CN112048781A - Degradable antibacterial flame-retardant PLA wig fiber and preparation method thereof - Google Patents
Degradable antibacterial flame-retardant PLA wig fiber and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41G—ARTIFICIAL FLOWERS; WIGS; MASKS; FEATHERS
- A41G3/00—Wigs
- A41G3/0083—Filaments for making wigs
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
- D01D5/092—Cooling filaments, threads or the like, leaving the spinnerettes in shafts or chimneys
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/096—Humidity control, or oiling, of filaments, threads or the like, leaving the spinnerettes
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
- D01D5/16—Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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Abstract
The invention provides degradable antibacterial flame-retardant PLA wig fibers, and relates to the technical field of simulation wigs. The wig fiber comprises the following components in percentage by weight: 80-90% of PLA, 5-8% of composite flame retardant, 3-6% of composite antibacterial agent, 0.5-1% of coloring agent, 0.6-2.2% of additive, 0.4-1.8% of dispersing agent and 0.5-1% of plasticizer. The composite flame retardant consists of three phosphorus flame retardants of APP, HPCP and DOPO-HQ, and a small amount of a flame retardant additive DCP is added, so that the flame retardant property of the flame retardant is remarkably improved, and the mechanical property of the flame retardant is ensured; the composite antibacterial agent consists of chitosan with good biocompatibility, tea polyphenol and triclocarban, so that the bacteriostatic rates of the composite antibacterial agent on staphylococcus aureus, escherichia coli and candida albicans can reach more than 95%, and the composite antibacterial agent shows excellent antibacterial performance. The wig fiber provided by the invention has the advantages of good smoothness and luster, excellent elasticity, strong wear resistance, environmental friendliness, degradability, antibacterial property, flame retardance and the like.
Description
Technical Field
The invention relates to the technical field of simulation wigs, in particular to degradable antibacterial flame-retardant PLA wig fibers and a preparation method thereof.
Background
With the rapid development of economy and the change of living habits of people, wigs become essential ornaments for pursuing individuation of people, great convenience is provided for people who are puzzled by hair problems, and meanwhile, with the development of cultural industries such as movies and TV, drama and the like, the demand of wigs is increasing day by day. The raw materials of wigs are generally derived from natural human hair and artificial wig fibers, and due to the scarcity of natural human hair resources, the artificial wig fibers are widely applied at home and abroad as substitutes of the natural human hair. At present, the existing artificial wig fiber is mainly prepared from polypropylene, polyvinyl chloride, polyester and the like as raw materials, the preparation process is complex, and the wig fiber prepared from the raw materials cannot be naturally degraded after being abandoned by a user, so that a large amount of accumulation can be caused for a long time. The existing treatment method is incineration activation, but the method can release greenhouse gases and toxic gases, and is not beneficial to human health and environmental development.
Biodegradable materials generally refer to polymeric materials that eventually break down into small molecules or contain water and carbon dioxide under natural or other specified processing conditions. The development and application of the method can reduce the dependence of the industry on petroleum products and avoid the damage to the environment. Polylactic acid Fiber (PLA Fiber) is short for PLA Fiber, belongs to 100 percent of bio-based synthetic Fiber, and is a renewable, green and 100 percent biodegradable synthetic Fiber material. The polylactic acid fiber is prepared from starch as basic raw material, which is mainly extracted from crops (such as corn), the extracted starch is converted into glucose under the action of enzyme or catalyst, the glucose is fermented by strains or microorganisms (mainly lactic acid bacteria) to form high-purity lactic acid, and then the high-purity lactic acid is subjected to polycondensation and melt spinning. Because the source of the fertilizer is easy to plant, the fertilizer does not need to use petroleumWood and can be decomposed into CO by the action of microorganisms2And water, the use process is nontoxic, and the natural environment cannot be seriously damaged. The polylactic acid is a nontoxic, nonirritating and plastic-processing-molded thermoplastic polyester, has the advantages of good transparency and high strength, has the same level of physical and mechanical properties as polystyrene, and becomes a fiber material with development prospect in the 21 st century. At present, polylactic acid fiber is mostly used for textile fabrics, sports goods, sanitary goods and the like, and the polylactic acid fiber is only used for preparing wig fiber in a few research reports.
As the wig can be directly or indirectly contacted with a human body in wearing and using processes, the wig needs to have good flame retardant property and antibacterial property to ensure the safety performance of the wig. Patent CN102926024A discloses degradable wig polylactic acid fiber and its production process, and the patent relates to wig fiber and has no antibacterial and flame retardant effect. PLA has poor flame retardant performance, the Limiting Oxygen Index (LOI) of the PLA is only about 20 percent, the UL-94 in a vertical combustion test can only reach a V-2 grade, and most of degradation products are combustible gases. In addition, the PLA can be quickly melted after being combusted, so that melt drops, secondary damage is caused, and casualties and economic loss are increased. In order to make PLA used for manufacturing wig fibers, it is necessary to modify PLA in a flame retardant manner to improve the flame retardant property and the anti-dripping property of the PLA. In recent years, halogen flame retardants have been dominant in the flame retardant market because of their relatively inexpensive raw materials and high flame retardant efficiency. However, halogen-based flame retardants release a large amount of hydrogen halide gas while retarding flame, have high corrosivity and often cause secondary damage, and thus halogen-free flame retardants are receiving more and more attention from people. The phosphorus flame retardant is the most environment-friendly flame retardant at present and is also a flame retardant type commonly used in PLA flame retardant research. In addition, various bacteria and molds, such as staphylococcus aureus, escherichia coli, and the like, exist in human living environments; under the environment of high temperature and high humidity, the microorganisms are easy to breed in large quantity, the temperature of the scalp is higher due to the fact that heat is not easy to dissipate after the wig is worn, and wig fibers are easy to degrade and discolor under the action of acid or alkaline metabolites of wig fibers, bacteria are bred, and certain skin diseases of a human body are easy to cause. Therefore, the production of the wig with strong antibacterial ability and health has practical significance.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a degradable antibacterial flame-retardant PLA wig fiber and a preparation method thereof, so that the wig fiber has environment-friendly and naturally degradable effects, can realize flame-retardant, anti-dripping and antibacterial effects, and enhances the safety performance of the wig fiber.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme:
a degradable antibacterial flame-retardant PLA wig fiber is prepared from the following components in percentage by weight: 80-90% of PLA, 5-8% of composite flame retardant, 3-6% of composite antibacterial agent, 0.5-1% of coloring agent, 0.6-2.2% of additive, 0.4-1.8% of dispersing agent and 0.5-1% of plasticizer.
The degradable antibacterial flame-retardant PLA wig fiber is further optimized by the following steps: the PAL has an intrinsic viscosity of 1.65-1.85 dl/g.
The degradable antibacterial flame-retardant PLA wig fiber is further optimized by the following steps: the composite flame retardant comprises the following components in parts by weight (4-5): (2.5-3): (1.5-2): (0.5-1) polyphosphoric acid, namely (APP), Hexaphenoxycyclophosphazene (HPCP), 10- (2, 5-dihydroxyphenyl) -10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO-HQ) and dicumyl peroxide (DCP).
The degradable antibacterial flame-retardant PLA wig fiber is further optimized by the following steps: the composite antibacterial agent comprises the following components in parts by weight (3-6): (2.5-4): (1.5-3) chitosan, tea polyphenol and triclocarban.
The degradable antibacterial flame-retardant PLA wig fiber is further optimized by the following steps: the coloring agent is toner, pigment or color master batch.
The degradable antibacterial flame-retardant PLA wig fiber is further optimized by the following steps: the additive is one or more of nano calcium carbonate, silicon dioxide, talcum powder, silicon micropowder, titanium dioxide and glass beads.
The degradable antibacterial flame-retardant PLA wig fiber is further optimized by the following steps: the dispersing agent is vinyl bis stearamide or polyethylene wax with the molecular weight of 2400-3200.
The degradable antibacterial flame-retardant PLA wig fiber is further optimized by the following steps: the plasticizer is acetyl tributyl citrate.
A preparation method of degradable antibacterial flame-retardant PLA wig fibers comprises the following steps:
(1) taking raw materials, 80-90% of PLA, 5-8% of composite flame retardant, 3-6% of composite antibacterial agent, 0.5-1% of coloring agent, 0.6-2.2% of additive, 0.4-1.8% of dispersant and 0.5-1% of plasticizer according to the weight ratio, and dehumidifying and drying the raw materials at the temperature of 80 ℃; the total time of dehumidification and drying is 8 hours, and the water content of the raw material is controlled within 50 ppm;
(2) putting the raw materials into a single screw rod extruder, carrying out spiral melt extrusion to obtain nascent fiber, wherein the aperture of a spinneret plate is 0.4-0.8mm, and the temperature of the extruder is 220-;
(3) cooling the nascent fiber by adopting a circular blowing or side blowing mode of 1-5 m or more, wherein the air temperature is 5-10 ℃;
(4) oiling the nascent fiber through an oiling roller, drafting the oiled nascent fiber through a drafting machine to obtain a tow after the drafting is finished, collecting the tow through a winding machine to obtain a fiber yarn roller, wherein the stretching temperature in the stretching process is 90-95 ℃, and the rotating speed is 600-650 m/min;
(5) putting a fiber yarn roller into a bundling frame, and enabling the yarn bundle to enter a heat setting box from the bundling frame through a traction roller to carry out a heat setting process, wherein the length of the heat setting box is 2-18 m, the working temperature of the heat setting machine is 165-175 ℃, the feeding speed of the yarn bundle is 2-5 m/min, and the retention time of the yarn bundle in the heat setting box is 10-15 min;
(6) after the heat setting process is finished, the degradable antibacterial flame-retardant PLA wig fiber can be obtained by winding and packaging the yarn through a yarn winding machine.
The preparation method of the degradable antibacterial flame-retardant PLA wig fiber is further optimized as follows: the oil agent adopted in the step (4) is one or more of polyether polymer, fatty acid polymer, organic amine salt compound and organic silicon;
the preparation method of the degradable antibacterial flame-retardant PLA wig fiber is further optimized as follows: the number of rollers of the drafting machine in the step (4) is 6-10 rollers, and the drafting ratio is 2.4-6.3 times.
(III) advantageous effects
The invention provides a degradable antibacterial flame-retardant PLA wig fiber and a preparation method thereof. PLA itself belongs to a flammable material, and a flame retardant needs to be additionally added to modify the PLA so as to achieve the purpose of flame retardance; although PLA has a certain antibacterial property, in practical applications, the antibacterial property of PLA cannot meet the standard of use, so that the PLA material is modified by adding an antibacterial agent to achieve the purpose of enhancing the antibacterial property. In the prior art, one antibacterial agent or flame retardant is mostly used for improving the performance of the fiber, and the effect is often not in an ideal state, so that the composite antibacterial agent and the composite flame retardant are reasonably compounded purposefully.
The phosphorus flame retardant is the most environment-friendly flame retardant at present and is also a flame retardant type commonly used in PLA flame retardant research. Therefore, the composite flame retardant provided by the invention consists of three phosphorus flame retardants of polyphosphoric Acid (APP), Hexaphenoxycyclophosphazene (HPCP) and 10- (2, 5-dihydroxyphenyl) -10-hydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO-HQ), the three phosphorus flame retardants are used together to play a synergistic effect, the flame retardant effect is played in two aspects of a coacervation phase and a gas phase, a small amount of dicumyl peroxide (DCP) serving as a flame retardant additive is added, and the mechanical property of wig fibers is ensured while the flame retardant property of the wig fibers is remarkably improved.
Because PLA has good biocompatibility, chitosan, tea polyphenol and triclocarban which have the same good biocompatibility are purposefully selected, and the three antibacterial agents are compounded and used together according to a reasonable proportion, so that the bacteriostasis rate of the wig fiber on staphylococcus aureus, escherichia coli and candida albicans can reach more than 95%, and the excellent antibacterial performance is shown.
The invention selects degradable PLA as the raw material, and adds the environment-friendly flame retardant and the natural antibacterial agent, so that the prepared wig fiber has the advantages of good smoothness and luster, excellent elasticity, strong wear resistance, environmental protection, antibiosis, flame retardance and the like.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but 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
A degradable antibacterial flame-retardant PLA wig fiber is prepared according to the following steps:
(1) taking raw materials according to the weight ratio, namely 90 percent of PLA, 5 percent of composite flame retardant, 3 percent of composite antibacterial agent, 0.5 percent of coloring agent, 0.6 percent of additive, 0.4 percent of dispersant and 0.5 percent of plasticizer, and dehumidifying and drying the raw materials at the temperature of 80 ℃; the total time of dehumidification and drying is 8 hours, and the water content of the raw material is controlled within 50 ppm;
wherein the intrinsic viscosity of PLA is 1.65 dl/g; the composite flame retardant comprises the following components in percentage by weight: 2.5: 1.5: 0.5 of APP, HPCP, DOPO-HQ and DCP; the composite antibacterial agent comprises the following components in percentage by weight: 2.5: 1.5 of chitosan, tea polyphenol and triclocarban; the coloring agent is black color master batch; the additive is silicon dioxide and talcum powder with the weight ratio of 1: 1; the dispersing agent is vinyl bis stearamide; the plasticizer is acetyl tributyl citrate.
(2) Putting the raw materials into a single screw rod extruder, carrying out spiral melt extrusion to obtain nascent fiber, wherein the aperture of a spinneret plate is 0.4mm, and the temperature of the extruder is 220 ℃;
(3) cooling the nascent fiber by adopting a 3-meter circular blowing or air measuring blowing mode, wherein the air temperature is 5-10 ℃;
(4) oiling the nascent fiber through an oiling roller, drafting the oiled nascent fiber through a drafting machine to obtain a tow after the drafting is finished, collecting the tow through a winding machine to obtain a fiber yarn roller, wherein the stretching temperature in the stretching process is 90 ℃, and the rotating speed is 600 m/min; wherein, the oiling agent is organic silicon; the number of rollers of the drafting machine is 10 rollers, and the drafting ratio is 6.3 times;
(5) putting a fiber yarn roller into a bundling frame, and enabling the yarn bundle to enter a heat setting box from the bundling frame through a traction roller to carry out a heat setting process, wherein the length of the heat setting box is 15 meters, the working temperature of the heat setting machine is 165 ℃, the feeding speed of the yarn bundle is 2m/min, and the retention time of the yarn bundle in the heat setting box is 10 minutes;
(6) after the heat setting process is finished, the degradable antibacterial flame-retardant PLA wig fiber can be obtained by winding and packaging the yarn through a yarn winding machine.
Example 2
A degradable antibacterial flame-retardant PLA wig fiber is different from the fiber in the embodiment 1:
taking raw materials according to the weight ratio, namely 90 percent of PLA, 5 percent of composite flame retardant, 3 percent of composite antibacterial agent, 0.5 percent of coloring agent, 0.6 percent of additive, 0.4 percent of dispersant and 0.5 percent of plasticizer, and dehumidifying and drying the raw materials at the temperature of 80 ℃; the total time of dehumidification and drying is 8 hours, and the water content of the raw material is controlled within 50 ppm;
wherein the intrinsic viscosity of PLA is 1.65 dl/g; the composite flame retardant consists of the following components in percentage by weight of 4: 3: 2: 1 of APP, HPCP, DOPO-HQ and DCP; the composite antibacterial agent comprises the following components in percentage by weight of 3: 4: 3, chitosan, tea polyphenol and triclocarban; the coloring agent is brown color master batch; the additive is nano calcium carbonate and talcum powder with the weight ratio of 1: 1; the dispersant is polyethylene wax with the molecular weight of 2800; the plasticizer is acetyl tributyl citrate.
The remaining preparation steps were the same as in example 1.
Example 3
A degradable antibacterial flame-retardant PLA wig fiber is prepared according to the following steps:
(1) taking raw materials, namely 80% of PLA, 8% of composite flame retardant, 6% of composite antibacterial agent, 1% of coloring agent, 2.2% of additive, 1.8% of dispersant and 1% of plasticizer according to the weight ratio, and dehumidifying and drying the raw materials at the temperature of 80 ℃; the total time of dehumidification and drying is 8 hours, and the water content of the raw material is controlled within 50 ppm;
wherein the intrinsic viscosity of PLA is 1.65 dl/g; the composite flame retardant comprises the following components in percentage by weight: 2.5: 1.5: 0.5 of APP, HPCP, DOPO-HQ and DCP; the composite antibacterial agent comprises the following components in percentage by weight: 2.5: 1.5 of chitosan, tea polyphenol and triclocarban; the coloring agent is black color master batch; the additive is silicon dioxide and talcum powder with the weight ratio of 1: 1; the dispersing agent is vinyl bis stearamide; the plasticizer is acetyl tributyl citrate.
(2) Putting the raw materials into a single-screw extruder, carrying out spiral melt extrusion to obtain nascent fiber, wherein the aperture of a spinneret plate is 0.8mm, and the temperature of the extruder is 235 ℃;
(3) cooling the nascent fiber by adopting a 3-meter circular blowing or air measuring blowing mode, wherein the air temperature is 5-10 ℃;
(4) oiling the nascent fiber through an oiling roller, drafting the oiled nascent fiber through a drafting machine to obtain a tow after the drafting is finished, collecting the tow through a winding machine to obtain a fiber yarn roller, wherein the stretching temperature in the stretching process is 95 ℃, and the rotating speed is 650 m/min; wherein, the oiling agent is organic silicon; the number of rollers of the drafting machine is 45 rollers, and the drafting ratio is 5.8 times;
(5) putting a fiber yarn roller into a bundling frame, and enabling the yarn bundle to enter a heat setting box from the bundling frame through a traction roller to carry out a heat setting process, wherein the length of the heat setting box is 18 meters, the working temperature of the heat setting machine is 175 ℃, the feeding speed of the yarn bundle is 5m/min, and the retention time of the yarn bundle in the heat setting box is 10 minutes;
(6) after the heat setting process is finished, the degradable antibacterial flame-retardant PLA wig fiber can be obtained by winding and packaging the yarn through a yarn winding machine.
Example 4
A degradable antibacterial flame-retardant PLA wig fiber is different from the fiber in the embodiment 3:
taking raw materials, namely 80% of PLA, 8% of composite flame retardant, 6% of composite antibacterial agent, 1% of coloring agent, 2.2% of additive, 1.8% of dispersant and 1% of plasticizer according to the weight ratio, and dehumidifying and drying the raw materials at the temperature of 80 ℃; the total time of dehumidification and drying is 8 hours, and the water content of the raw material is controlled within 50 ppm;
wherein the intrinsic viscosity of PLA is 1.65 dl/g; the composite flame retardant consists of the following components in percentage by weight of 4: 3: 2: 1 of APP, HPCP, DOPO-HQ and DCP; the composite antibacterial agent comprises the following components in percentage by weight of 3: 4: 3, chitosan, tea polyphenol and triclocarban; the coloring agent is brown color master batch; the additive is nano calcium carbonate and talcum powder with the weight ratio of 1: 1; the dispersant is polyethylene wax with the molecular weight of 2800; the plasticizer is acetyl tributyl citrate.
The remaining preparation steps were the same as in example 3.
Example 5
A degradable antibacterial flame-retardant PLA wig fiber is different from the fiber in the embodiment 3:
taking raw materials according to the weight ratio, 85% of PLA, 7% of composite flame retardant, 4% of composite antibacterial agent, 0.8% of coloring agent, 1.2% of additive, 1.4% of dispersant and 0.6% of plasticizer, and dehumidifying and drying the raw materials at the temperature of 80 ℃; the total time of dehumidification and drying is 8 hours, and the water content of the raw material is controlled within 50 ppm;
wherein the intrinsic viscosity of PLA is 1.65 dl/g; the composite flame retardant consists of the following components in percentage by weight of 4.6: 2.7: 1.9: 0.8 of APP, HPCP, DOPO-HQ and DCP; the composite antibacterial agent comprises the following components in percentage by weight: 3: 2, chitosan, tea polyphenol and triclocarban; the coloring agent is red color master batch; the additive is glass beads; the dispersant is polyethylene wax with the molecular weight of 3200; the plasticizer is acetyl tributyl citrate.
The remaining preparation steps were the same as in example 3.
Example 6
A degradable antibacterial flame-retardant PLA wig fiber is different from the fiber in the embodiment 3:
taking raw materials according to the weight ratio, namely 83 percent of PLA, 6.9 percent of composite flame retardant, 4.9 percent of composite antibacterial agent, 0.9 percent of coloring agent, 2 percent of additive, 1.5 percent of dispersant and 0.8 percent of plasticizer, and dehumidifying and drying the raw materials at the temperature of 80 ℃; the total time of dehumidification and drying is 8 hours, and the water content of the raw material is controlled within 50 ppm;
wherein the intrinsic viscosity of PLA is 1.65 dl/g; the composite flame retardant consists of the following components in percentage by weight of 4.4: 2.9: 2: 0.7 of APP, HPCP, DOPO-HQ and DCP; the composite antibacterial agent comprises the following components in percentage by weight of 4.8: 3.4: 1.8 of chitosan, tea polyphenol and triclocarban; the coloring agent is red color master batch; the additive is silicon micropowder; the dispersing agent is vinyl bis stearamide; the plasticizer is acetyl tributyl citrate.
The remaining preparation steps were the same as in example 3.
The diameters, breaking strengths and breaking elongations of the degradable antibacterial flame-retardant PLA wig fibers obtained in examples 1-6 were measured, the quality, the flexibility and the combing performance of equivalent nylon wig fibers were evaluated through sensory evaluation, and the results are shown in Table 1 by taking the straight hair of a real person as a comparative example.
TABLE 1 results of various property tests on real hair and samples of examples 1-6 of the present invention
As can be seen from table 1, the wig fibers of the present invention obtained in examples 1 to 6 have no significant difference in quality compared to the straight hair of a real person, and have insignificant difference in breaking strength, elongation at break, flexibility, combing property, and the like compared to the straight hair of a real person, and are slightly improved, which indicates that the antibacterial flame retardant nylon wig fibers of the present invention have the advantages of good flexibility, excellent elasticity, strong wear resistance, and the like.
To further illustrate the antibacterial and flame retardant properties of the degradable antibacterial flame retardant PLA wig fibers obtained in examples 1-6, the samples of examples 1-6 were subjected to antibacterial property test, Limiting Oxygen Index (LOI) test and vertical burning test (UL 94).
The test method comprises the following steps:
and (3) testing antibacterial performance: and (3) placing the bacterial liquid with a certain concentration on the sample, culturing for a certain time, and measuring the number of the residual bacteria to obtain the antibacterial rate of the composite material. The strains are respectively staphylococcus aureus, escherichia coli and candida albicans.
Limiting oxygen index test (LOI): the oxygen index test is carried out according to the national standard GB/T5454-1997.
Vertical burning test (UL 94): the vertical burn test was determined according to GB/T5455-2004. The test grades are HB, V-2, V-1 and V-0.
The antimicrobial and flame retardant properties of the samples of examples 1-6 are shown in table 2.
TABLE 2 antibacterial and flame retardant Properties of the samples of examples 1-6
As can be seen from the results in Table 2, the wig fibers obtained in examples 1-6 all achieved V-0 rating under the UL-94 vertical burning test method; the limit oxygen index can reach 34-36% under the limit oxygen index measurement, the flame-retardant material belongs to a flame-retardant material, and after the tow is ignited for 10 seconds twice, the flame is extinguished within 30 seconds, and no drop is generated. The obtained wig fiber has excellent flame retardant property. Meanwhile, the wig fibers obtained in the embodiments 1-6 added with the antibacterial agent in a reasonable ratio have the bacteriostasis rate of over 95 percent on staphylococcus aureus, escherichia coli and candida albicans, and show excellent antibacterial performance. The results show that the wig fiber has very excellent flame retardant property and antibacterial property, and can greatly ensure the safety of users.
The technical key point of the degradable antibacterial PLA flame-retardant wig fiber provided by the invention is the use of a composite antibacterial agent and a composite flame retardant, in the prior art, a certain antibacterial agent or flame retardant is mostly used for improving the performance of the fiber, and the effect often does not reach an ideal state. To further illustrate the formulation advantages of the present invention, various formulations are provided below along with the limiting oxygen index test (LOI), the vertical burn test (UL 94), and the antimicrobial performance test of the present invention.
1 LOI and UL 94 testing
Sample preparation: taking raw materials according to the weight ratio, namely 90 percent of PLA, 5 percent of composite flame retardant, 3 percent of composite antibacterial agent, 0.5 percent of coloring agent, 0.6 percent of additive, 0.4 percent of dispersant and 0.5 percent of plasticizer, and dehumidifying and drying the raw materials at the temperature of 80 ℃; the total time of dehumidification and drying is 8 hours, and the water content of the raw material is controlled within 50 ppm; wherein the intrinsic viscosity of PLA is 1.65 dl/g; the composite flame retardant consists of APP, HPCP, DOPO-HQ and/or DCP in a certain weight ratio (see Table 3); the composite antibacterial agent comprises the following components in percentage by weight: 2.5: 1.5 of chitosan, tea polyphenol and triclocarban; the coloring agent is black color master batch; the additive is silicon dioxide and talcum powder with the weight ratio of 1: 1; the dispersing agent is vinyl bis stearamide; the plasticizer was acetyl tributyl citrate and was prepared according to the procedure shown in example 1 to obtain groups 1-8 wig fibers, respectively.
The test method comprises the following steps:
limiting oxygen index test (LOI): the oxygen index test is carried out according to the national standard GB/T5454-1997.
Vertical burning test (UL 94): the vertical burn test was determined according to GB/T5455-2004. The test grades are divided into NR, V-2, V-1 and V-0.
The flame retardant properties of the samples from groups 1-8 are shown in Table 3.
Flame retardant Properties of samples in groups 31-8 of Table
PLA itself belongs to inflammable materials, needs to be additionally added with a flame retardant to modify the PLA so as to achieve the purpose of flame retardance. Therefore, the flame retardant performance of the wig fiber prepared without adding a flame retardant is not compared. In recent years, halogen flame retardants have been dominant in the flame retardant market because of their relatively inexpensive raw materials and high flame retardant efficiency. However, halogen-based flame retardants release a large amount of hydrogen halide gas while retarding flame, have high corrosivity and often cause secondary damage, and thus halogen-free flame retardants are receiving more and more attention from people. The phosphorus flame retardant is the most environment-friendly flame retardant at present and is also a flame retardant type commonly used in PLA flame retardant research. Three phosphorus flame retardants of polyphosphoric Acid (APP), Hexaphenoxycyclophosphazene (HPCP) and 10- (2, 5-dihydroxyphenyl) -10-hydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO-HQ) are purposefully selected, and the flame retardant effects of the three flame retardants which are used independently and compounded are tested, and the results are shown in Table 3.
Dicumyl peroxide (DCP) is commonly used as a vulcanizer, a crosslinking agent, a curing agent, and a flame retardant additive for polymeric materials. Comparing group 1 and group 2, it can be seen that the addition of DCP has no influence on the flame retardant performance of the fiber, and the limiting oxygen indexes of group 1 and group 2 are 35% and 34%, respectively, with no obvious difference; however, the wig fibers need to have good mechanical properties due to the limitation of the application, the elongation at break can be obviously reduced by adding a small amount of DCP, and the mechanical properties of the wig fibers in the group 1 are obviously higher than those of the wig fibers in the group 2. Comparing the elongation at break of the groups 1 and 3-8, it can be seen that the difference in elongation at break between the groups is not significant, and the result shows that the good mechanical properties of wig fibers can be maintained by adding a small amount of DCP regardless of the composition of the flame retardant.
The limited oxygen indexes of the wig fibers of 3-8 groups are all above 29%, which shows that the flame retardant property of the fibers is obviously improved by adding the flame retardant, and the prepared wig fibers are all flame retardant substances. The LOI of 3-5 groups is 31-32%, the LOI of 6-8 groups is 29-30%, and comparison shows that the flame retardant effect of one flame retardant used alone is not obvious when two flame retardants are used in a compounding way. Compared with the groups 3-8, the LOI of the group 1 is as high as 35%, the LOI reaches the V-0 grade under the UL-94 vertical combustion test method, and is obviously higher than the LOI of the group 3-8, and the LOI is obviously different. The results show that the polyphosphoric acid plays a synergistic effect by using three phosphorus flame retardants of (APP), Hexaphenoxycyclophosphazene (HPCP) and 10- (2, 5-dihydroxyphenyl) -10-hydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO-HQ) together, and plays a flame retardant role in both condensed phase and gas phase, and a small amount of dicumyl peroxide (DCP) is added, so that the mechanical property of the wig fiber is ensured while the flame retardant property of the wig fiber is remarkably improved.
2 test of antibacterial Properties
Sample preparation: taking raw materials according to the weight ratio, namely 90 percent of PLA, 5 percent of composite flame retardant, 3 percent of composite antibacterial agent, 0.5 percent of coloring agent, 0.6 percent of additive, 0.4 percent of dispersant and 0.5 percent of plasticizer, and dehumidifying and drying the raw materials at the temperature of 80 ℃; the total time of dehumidification and drying is 8 hours, and the water content of the raw material is controlled within 50 ppm; wherein the intrinsic viscosity of PLA is 1.65 dl/g; the composite flame retardant comprises the following components in percentage by weight: 2.5: 1.5: 0.5 of APP, HPCP, DOPO-HQ and DCP; chitosan, tea polyphenol and/or triclocarban in a certain weight ratio of the composite antibacterial agent (see table 4); the coloring agent is black color master batch; the additive is silicon dioxide and talcum powder with the weight ratio of 1: 1; the dispersing agent is vinyl bis stearamide; the plasticizer was acetyl tributyl citrate and was prepared according to the procedure shown in example 1 to obtain groups 1-7 wig fibers, respectively.
The test method comprises the following steps: and (3) placing the bacterial liquid with a certain concentration on the sample, culturing for a certain time, and measuring the number of the residual bacteria to obtain the antibacterial rate of the composite material. The strains are respectively staphylococcus aureus, escherichia coli and candida albicans.
The antimicrobial properties of the samples from groups 1-7 are shown in Table 4.
Antibacterial Properties of samples of groups 41-7 in Table
PLA itself has a certain antibacterial property, but in practical applications, the antibacterial property of PLA itself cannot meet the standard of use, so that the PLA material is generally modified by adding an antibacterial agent to achieve the purpose of enhancing the antibacterial property. Therefore, the antibacterial performance of the wig fiber prepared without adding the antibacterial agent is not compared. Because PLA has good biocompatibility, chitosan, tea polyphenol and triclocarban which also have good biocompatibility are purposefully selected and tested for the antibacterial effect when being used alone or compounded, and the results are shown in Table 4.
Comparing the bacteriostatic rates of the 5-7 groups, the chitosan, the tea polyphenol and the triclocarban can increase the antibacterial performance of the wig fiber, and the bacteriostatic rates of the chitosan, the tea polyphenol and the triclocarban on staphylococcus aureus, escherichia coli and candida albicans are about 71-77%, wherein the bacteriostatic performance of the chitosan is higher than that of the tea polyphenol and the triclocarban; comparing the bacteriostatic rates of the groups 2-4 and the groups 5-7, the bacteriostatic rate of the three antibacterial agents compounded in pairs is higher than that of a single antibacterial agent, the bacteriostatic rate of the three antibacterial agents on staphylococcus aureus, escherichia coli and candida albicans is improved by about 10-15%, the bacteriostatic rate of the groups 2 and 3 containing chitosan on staphylococcus aureus, escherichia coli and candida albicans is obviously higher than that of the group 4, and the result shows that the chitosan plays a main bacteriostatic role; comparing the bacteriostatic rates of the groups 1 and 2-7, the chitosan, the tea polyphenol and the triclocarban are compounded together for use, so that the bacteriostatic rate of the wig fiber on staphylococcus aureus, escherichia coli and candida albicans can reach more than 95%, and excellent antibacterial performance is shown; the results are combined to show that the wig fiber has obvious bacteriostatic effect on staphylococcus aureus, escherichia coli and candida albicans by adding three antibacterial agents of chitosan, tea polyphenol and triclocarban in a reasonable ratio and the combined action of the antibacterial agents.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The utility model provides a fire-retardant PLA wig fibre of degradable antibiotic which characterized in that: the composition is prepared from the following components in percentage by weight: 80-90% of PLA, 5-8% of composite flame retardant, 3-6% of composite antibacterial agent, 0.5-1% of coloring agent, 0.6-2.2% of additive, 0.4-1.8% of dispersing agent and 0.5-1% of plasticizer.
2. The degradable antibacterial flame-retardant PLA wig fiber according to claim 1, wherein: the PAL has an intrinsic viscosity of 1.65-1.85 dl/g.
3. The degradable antibacterial flame-retardant PLA wig fiber according to claim 1, wherein: the composite flame retardant comprises the following components in parts by weight (4-5): (2.5-3): (1.5-2): (0.5-1) polyphosphoric acid, namely (APP), Hexaphenoxycyclophosphazene (HPCP), 10- (2, 5-dihydroxyphenyl) -10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO-HQ) and dicumyl peroxide (DCP).
4. The degradable antibacterial flame-retardant PLA wig fiber according to claim 1, wherein: the composite antibacterial agent comprises the following components in parts by weight (3-6): (2.5-4): (1.5-3) chitosan, tea polyphenol and triclocarban.
5. The degradable antibacterial flame-retardant PLA wig fiber according to claim 1, wherein: the coloring agent is toner, pigment or color master batch.
6. The degradable antibacterial flame-retardant PLA wig fiber according to claim 1, wherein: the additive is one or more of nano calcium carbonate, silicon dioxide, talcum powder, silicon micropowder, titanium dioxide and glass beads.
7. The degradable antibacterial flame-retardant PLA wig fiber according to claim 1, wherein: the dispersing agent is vinyl bis stearamide or polyethylene wax with the molecular weight of 2400-3200.
8. The degradable antibacterial flame-retardant PLA wig fiber according to claim 1, wherein: the plasticizer is acetyl tributyl citrate.
9. A preparation method of degradable antibacterial flame-retardant PLA wig fibers comprises the following steps:
(1) taking raw materials, 80-90% of PLA, 5-8% of composite flame retardant, 3-6% of composite antibacterial agent, 0.5-1% of coloring agent, 0.6-2.2% of additive, 0.4-1.8% of dispersant and 0.5-1% of plasticizer according to the weight ratio, and dehumidifying and drying the raw materials at the temperature of 80 ℃; the total time of dehumidification and drying is 8 hours, and the water content of the raw material is controlled within 50 ppm;
(2) putting the raw materials into a single screw rod extruder, carrying out spiral melt extrusion to obtain nascent fiber, wherein the aperture of a spinneret plate is 0.4-0.8mm, and the temperature of the extruder is 220-;
(3) cooling the nascent fiber by adopting a cooling ring blowing or measuring blowing mode of 1-5 meters or more, wherein the air temperature is 5-10 ℃;
(4) oiling the nascent fiber through an oiling roller, drafting the oiled nascent fiber through a drafting machine to obtain a tow after the drafting is finished, collecting the tow through a winding machine to obtain a fiber yarn roller, wherein the stretching temperature in the stretching process is 90-95 ℃, and the rotating speed is 600-650 m/min; the number of rollers of the drafting machine is 6-10, and the drafting ratio is 2.4-6.3 times;
(5) putting a fiber yarn roller into a bundling frame, and enabling the yarn bundle to enter a heat setting box from the bundling frame through a traction roller to carry out a heat setting process, wherein the length of the heat setting box is 2-18 m, the working temperature of the heat setting machine is 165-175 ℃, the feeding speed of the yarn bundle is 2-5 m/min, and the retention time of the yarn bundle in the heat setting box is 10-15 min;
(6) after the heat setting process is finished, the degradable antibacterial flame-retardant PLA wig fiber can be obtained by winding and packaging the yarn through a yarn winding machine.
10. The preparation method of the degradable antibacterial flame-retardant PLA wig fiber according to claim 2, characterized in that: the oil agent adopted in the step (4) is one or more of polyether polymer, fatty acid polymer, organic amine salt compound and organic silicon.
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