CN111691006A - Medical antibacterial ES fiber and preparation process thereof - Google Patents
Medical antibacterial ES fiber and preparation process thereof Download PDFInfo
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- CN111691006A CN111691006A CN202010742121.9A CN202010742121A CN111691006A CN 111691006 A CN111691006 A CN 111691006A CN 202010742121 A CN202010742121 A CN 202010742121A CN 111691006 A CN111691006 A CN 111691006A
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
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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
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
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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
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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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- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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Abstract
The invention discloses a medical antibacterial ES fiber and a preparation process thereof. The leather layer material comprises 6-9 parts of leather layer resin, 2-3 parts of auxiliary agent and 0.8-1.5 parts of antibacterial agent; the core layer material comprises 6-9 parts of core layer resin, 2-3 parts of auxiliary agent and 0.8-1.5 parts of antibacterial agent. The preparation process comprises the steps of preparing the antibacterial agent, preparing the skin layer material and the core layer material, and carrying out mixed spinning on the skin layer material and the core layer material to obtain a finished product. The antibacterial agent is prepared by mixing modified Chinese juniper oil and nano core-shell particles in a mass ratio of 1:1, wherein the modified Chinese juniper oil is mainly prepared by reacting Chinese juniper oil, mesoporous silica, 3-aminopropyltriethoxysilane and polyacrylic acid; the nano core-shell particles are mainly prepared from silver nitrate and ferric nitrate. The medical antibacterial ES fiber prepared by the invention has strong bacteriostatic activity and can resist bacteria for a long time, and the problem of weak antibacterial effect caused by volatilization of the Chinese juniper oil is solved.
Description
Technical Field
The invention belongs to the technical field of fiber manufacturing, and particularly relates to a medical antibacterial ES fiber and a preparation process thereof.
Background
The ES fiber is a sheath-core composite fiber obtained by successfully combining a low-melting-point component and a high-melting-point component on one monofilament, has excellent heat bonding characteristics, greatly enriches the product varieties in the field of non-woven fabrics, and optimizes the quality of non-woven products. The low-melting point fiber in the ES fiber is melted under the heat treatment condition higher than the melting point of the ES fiber and is bonded with other materials, so that the non-woven fabric without using a binder can be formed. The first generation ES fibers were successfully developed by japan wisdom corporation with a sheath layer of PE (polyethylene) and a core layer of PP (polypropylene). PE/PET (polyethylene/polyester) composite ES fibers have been developed with a sheath layer of PE and a core layer of PET (polyester).
Because the ES fiber is a clean fiber without using adhesive, the ES fiber is widely applied to the covering of sanitary products and medical surgical products. Although the existing ES fiber reaches the quality standard of sanitary products and medical operations and has great advantages in safety, heat resistance, durability and mechanical properties, the durable antibacterial property of the ES fiber is required to be improved as a medical product.
Disclosure of Invention
The invention aims to provide a medical antibacterial ES fiber and a preparation process thereof, and aims to solve the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme: a medical antibacterial ES fiber is a sheath-core fiber and is prepared by mixing and spinning a sheath material and a core material; the leather layer material comprises the following raw materials, by weight, 6-9 parts of leather layer resin, 2-3 parts of an auxiliary agent and 0.8-1.5 parts of an antibacterial agent. The core layer material comprises, by weight, 6-9 parts of core layer resin, 2-3 parts of an auxiliary agent and 0.8-1.5 parts of an antibacterial agent.
The antibacterial agent is prepared by mixing modified Chinese juniper oil and nano core-shell particles, and the mass ratio of the modified Chinese juniper oil to the nano core-shell particles is 1: 1. The modified Chinese juniper oil is mainly prepared by reacting Chinese juniper oil, mesoporous silica, 3-aminopropyl triethoxysilane and polyacrylic acid; the nano core-shell particles are mainly prepared from silver nitrate and ferric nitrate.
The resin of the skin layer is polyethylene resin, and the melt index is 10-40g/10 min; the core layer resin is polyethylene terephthalate or polypropylene resin, and the melt index is 10-40g/10 min.
The auxiliary agent comprises 0.7 part of antioxidant, 0.5 part of dispersant, 0.4 part of coupling agent and 0.4 part of antistatic agent; the antioxidant is a mixture of hindered phenol antioxidant and phosphite ester antioxidant, the dispersant is succinimide, the coupling agent is any one of stearic acid, calcium stearate and silane coupling agent, and the antistatic agent is a mixture of glycerol trilaurate and ethoxylated alkyl acid.
A preparation process of medical antibacterial ES fiber comprises the following steps; (1) an antibacterial agent; (2) preparing a leather material; (3) preparing a core layer material; (4) and mixing and spinning to obtain the medical antibacterial ES fiber.
A preparation process of medical antibacterial ES fiber comprises the following steps;
(1) adding tetraethyl orthosilicate, ammonium bromide and ammonia water into mesoporous silica, mixing, stirring, heating, dropwise adding 3-aminopropyltriethoxysilane, stirring, reacting, filtering, washing with an absolute ethanol solution, and drying to obtain a substance A; dissolving polyacrylic acid in hydrochloric acid solution, stirring, adding N-hydroxysuccinimide and the substance A, stirring, filtering to remove solid phase, and drying to obtain a substance B; mixing the Chinese juniper oil with the substance B, filtering, and drying to obtain modified Chinese juniper oil.
Preparing nano core-shell particles; mixing silver nitrate solution, sodium chloride and ferric nitrate, adding ethylene glycol, performing ultrasonic dispersion, heating reaction, performing centrifugal separation, washing with absolute ethyl alcohol, performing vacuum drying, and grinding to obtain the nano core-shell particles. Mixing the modified Chinese juniper oil and the nano core-shell particles, performing ultrasonic dispersion, and performing vacuum drying to obtain the antibacterial agent.
The Chinese juniper oil is distillate of Thujopsis dolabrata, and its main ingredient is 4-isopropyl-2-hydroxy cycloheptyl-2, 4, 6-caryophyllene-1-ketone, which is a natural high-efficiency antibacterial agent; has killing effect on gram-positive bacteria, gram-negative bacteria, etc., and has stronger antifungal property on fungi. The technical scheme of the invention adopts a silane coupling agent and mesoporous silica to perform polycondensation reaction to form aminated mesoporous silica, acrylic acid is grafted to form a molecular carrier with large specific surface area and good compatibility, and the treated mesoporous silica carries out load coating on the Chinese juniper oil, so that the volatilization of the Chinese juniper oil is reduced, the molecular stability of the Chinese juniper oil is improved, and the Chinese juniper oil has long-acting antibacterial and bactericidal effects. Silver nitrate and ferric nitrate react to form nano core-shell particles taking silver as a core and ferroferric oxide as a shell; the nano core-shell particle can effectively solve the agglomeration phenomenon of silver particles, and simultaneously, the specific surface area of the silver particles in the ES fiber is increased to achieve a stronger antibacterial effect. The nanometer nuclear shell particles are mixed with the modified Chinese juniper oil to generate mutual synergistic effect so as to improve the antibacterial property of the ES fiber, and particularly, the antibacterial agent has strong killing effect on gram-negative bacteria and gram-positive bacteria and strong resistance to fungi. Therefore, the ES fiber prepared by the technical scheme has excellent antibacterial and bacteriostatic properties, and is particularly suitable for preparing medical operation materials and medical wiping and coating materials.
(2) Mixing 6-9 parts of polyethylene resin, 2-3 parts of auxiliary agent and 0.8-1.5 parts of antibacterial agent, and stirring at 63-67 ℃ for 40-50min to obtain a skin layer mixture.
(3) 6-9 parts of PET resin, 2-3 parts of auxiliary agent and 0.8-1.5 parts of antibacterial agent are mixed, and stirred for 40-50min at the temperature of 80-90 ℃ to obtain a core layer mixture.
(4) And (3) respectively adding the cortex layer mixture prepared in the step (2) and the core layer mixture prepared in the step (3) into a spinning machine according to a proportion, melting, co-extruding, spinning, water-cooling, drafting, drying and cutting to obtain the ES fiber.
A preparation process of medical antibacterial ES fiber comprises the following steps;
(1) adding tetraethyl orthosilicate, ammonium bromide and ammonia water into mesoporous silica, mixing, stirring, heating to 60 ℃, dropwise adding 3-aminopropyltriethoxysilane, stirring, reacting for 6-7h, filtering, washing with an absolute ethanol solution, and drying to obtain a substance A; dissolving polyacrylic acid in hydrochloric acid solution, stirring, adding N-hydroxysuccinimide and the substance A, stirring, filtering to remove solid phase, and drying to obtain a substance B; mixing the Chinese juniper oil with the substance B, ultrasonically dispersing for 20-30min, filtering, and drying to obtain modified Chinese juniper oil;
preparing nano core-shell particles; mixing a silver nitrate solution, sodium chloride and ferric nitrate, adding ethylene glycol, performing ultrasonic dispersion, heating to 205-215 ℃, reacting for 6-8h, performing centrifugal separation, washing with absolute ethyl alcohol, performing vacuum drying, and grinding to obtain nano core-shell particles; mixing the modified Chinese juniper oil and the nano core-shell particles, performing ultrasonic dispersion, and performing vacuum drying to obtain an antibacterial agent;
(2) mixing 6-9 parts of polyethylene resin, 2-3 parts of auxiliary agent and 0.8-1.5 parts of antibacterial agent, and stirring at 63-67 ℃ for 40-50min to obtain a skin layer mixture;
(3) mixing 6-9 parts of PET resin, 2-3 parts of auxiliary agent and 0.8-1.5 parts of antibacterial agent, and stirring at 80-90 ℃ for 40-50min to obtain a core layer mixture;
(4) mixing the skin layer material prepared in the step (2) and the core layer material prepared in the step (3) and adding the mixture into a spinning machine, wherein the mass ratio of the skin layer mixture to the core layer mixture is 3: 2; melting for 40-50min at the temperature of 185-195 ℃, co-extruding, spinning, water-cooling, drafting, drying and cutting to obtain the medical antibacterial ES fiber finished product.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the antibacterial agent formed by mixing the modified Chinese juniper oil and the nano core-shell particles is adopted to modify the sheath material and the core material, and the ES fiber formed after mixed spinning has excellent antibacterial and bacteriostatic properties; especially has strong killing effect on gram-negative bacteria and gram-positive bacteria and excellent performance of inhibiting fungi; is particularly suitable for preparing medical operation materials, medical wiping materials, coating materials and the like.
The specific implementation mode is as follows:
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
A medical antibacterial ES fiber is a sheath-core fiber, which is prepared by mixing and spinning a sheath material and a core material; the leather layer material comprises the following raw material components, by weight, 6 parts of leather layer resin, 2 parts of auxiliary agent and 0.8 part of antibacterial agent; the core layer material comprises the following raw material components, by weight, 6 parts of core layer resin, 2 parts of an auxiliary agent and 0.8 part of an antibacterial agent.
The antibacterial agent is prepared by mixing modified Chinese juniper oil and nano core-shell particles, and the mass ratio of the modified Chinese juniper oil to the nano core-shell particles is 1: 1.
The auxiliary agent comprises 0.7 part of antioxidant, 0.5 part of dispersant, 0.4 part of coupling agent and 0.4 part of antistatic agent.
A preparation process of medical antibacterial ES fiber comprises the following steps;
(1) adding tetraethyl orthosilicate, ammonium bromide and ammonia water into mesoporous silica, mixing, stirring, heating to 60 ℃, dropwise adding 3-aminopropyltriethoxysilane, stirring, reacting for 6 hours, filtering, washing with an absolute ethanol solution, and drying to obtain a substance A; dissolving polyacrylic acid in hydrochloric acid solution, stirring, adding N-hydroxysuccinimide and the substance A, stirring, filtering to remove solid phase, and drying to obtain a substance B; mixing the Chinese juniper oil with the substance B, ultrasonically dispersing for 20min, filtering, and drying to obtain modified Chinese juniper oil;
preparing nano core-shell particles, mixing silver nitrate solution, sodium chloride and ferric nitrate, and adding ethylene glycol, wherein the silver nitrate accounts for 2.71 wt%, the sodium chloride accounts for 1.55 wt%, the ferric nitrate accounts for 5.7%, and the ethylene glycol accounts for 1.2%. Performing ultrasonic dispersion for 15min, heating to 205 ℃, reacting for 6h, performing centrifugal separation, washing with absolute ethyl alcohol, drying in vacuum, and grinding to obtain nano core-shell particles; mixing the modified Chinese juniper oil and the nano core-shell particles, performing ultrasonic dispersion, and performing vacuum drying to obtain an antibacterial agent;
(2) mixing 6 parts of polyethylene resin, 2 parts of auxiliary agent and 0.8 part of antibacterial agent, and stirring for 40min at 63 ℃ to obtain a skin material;
(3) mixing 6 parts of PET resin, 2 parts of auxiliary agent and 0.8 part of antibacterial agent, and stirring for 40min at the temperature of 80 ℃ to obtain a skin material;
(4) mixing the sheath layer material prepared in the step (2) and the core layer material prepared in the step (3) and adding the mixture into a spinning machine, wherein the mass ratio of the sheath layer material to the core layer material is 3: 2; melting for 40min at 185 ℃, extruding under high pressure, spinning, water cooling, drafting, drying and cutting to obtain the finished product of the medical antibacterial ES fiber.
Example 2
A medical antibacterial ES fiber is a sheath-core fiber, which is prepared by mixing and spinning a sheath material and a core material; the leather layer material comprises 7 parts of leather layer resin, 2.5 parts of auxiliary agent and 1.1 parts of antibacterial agent according to parts by weight; the core layer material comprises the following raw material components, by weight, 7 parts of core layer resin, 2.5 parts of an auxiliary agent and 1.1 parts of an antibacterial agent.
The antibacterial agent is prepared by mixing modified Chinese juniper oil and nano core-shell particles, and the mass ratio of the modified Chinese juniper oil to the nano core-shell particles is 1: 1.
The auxiliary agent comprises 0.7 part of antioxidant, 0.5 part of dispersant, 0.4 part of coupling agent and 0.4 part of antistatic agent.
A preparation process of medical antibacterial ES fiber comprises the following steps;
(1) adding tetraethyl orthosilicate, ammonium bromide and ammonia water into mesoporous silica, mixing, stirring, heating to 60 ℃, dropwise adding 3-aminopropyltriethoxysilane, stirring, reacting for 6.5 hours, filtering, washing with an absolute ethanol solution, and drying to obtain a substance A; dissolving polyacrylic acid in hydrochloric acid solution, stirring, adding N-hydroxysuccinimide and the substance A, stirring, filtering to remove solid phase, and drying to obtain a substance B; mixing the Chinese juniper oil with the substance B, ultrasonically dispersing for 25min, filtering, and drying to obtain modified Chinese juniper oil;
mixing silver nitrate solution, sodium chloride and ferric nitrate, and adding ethylene glycol, wherein the silver nitrate is 4 wt%, the sodium chloride is 2.06 wt%, the ferric nitrate is 5.12%, and the ethylene glycol is 0.8%. Performing ultrasonic dispersion, heating to 212 ℃, reacting at high temperature for 7 hours, performing centrifugal separation, washing with absolute ethyl alcohol, drying in vacuum, and grinding to obtain nano core-shell particles; mixing the modified Chinese juniper oil and the nano core-shell particles, performing ultrasonic dispersion, and performing vacuum drying to obtain an antibacterial agent;
(2) mixing polyethylene resin, an auxiliary agent and an antibacterial agent, and stirring for 47min at the temperature of 65 ℃ to obtain a skin material;
(3) mixing PET resin, an auxiliary agent and an antibacterial agent 0, and stirring for 46min at 83 ℃ to obtain a skin material;
(4) mixing the sheath layer material prepared in the step (2) and the core layer material prepared in the step (3) and adding the mixture into a spinning machine, wherein the mass ratio of the sheath layer material to the core layer material is 3: 2; melting for 43min at 190 deg.C, extruding under high pressure, spraying, water cooling, drafting, oven drying, and cutting to obtain the final product.
Example 3
A medical antibacterial ES fiber is a sheath-core fiber, which is prepared by mixing and spinning a sheath material and a core material; the leather layer material comprises the following raw material components, by weight, 9 parts of leather layer resin, 3 parts of auxiliary agent and 1.5 parts of antibacterial agent; the core layer material comprises the following raw material components, by weight, 9 parts of core layer resin, 3 parts of an auxiliary agent and 1.5 parts of an antibacterial agent.
The antibacterial agent is prepared by mixing modified Chinese juniper oil and nano core-shell particles, and the mass ratio of the modified Chinese juniper oil to the nano core-shell particles is 1: 1.
The auxiliary agent comprises 0.7 part of antioxidant, 0.5 part of dispersant, 0.4 part of coupling agent and 0.4 part of antistatic agent.
A preparation process of medical antibacterial ES fiber comprises the following steps;
(1) adding tetraethyl orthosilicate, ammonium bromide and ammonia water into mesoporous silica, mixing, stirring, heating to 60 ℃, dropwise adding 3-aminopropyltriethoxysilane, stirring, reacting for 7 hours, filtering, washing with an absolute ethanol solution, and drying to obtain a substance A; dissolving polyacrylic acid in hydrochloric acid solution, stirring, adding N-hydroxysuccinimide and the substance A, stirring, filtering to remove solid phase, and drying to obtain a substance B; mixing the Chinese juniper oil with the substance B, ultrasonically dispersing for 30min, filtering, and drying to obtain modified Chinese juniper oil;
mixing silver nitrate solution, sodium chloride and ferric nitrate, and adding glycol, wherein the silver nitrate accounts for 1.71 wt%, the sodium chloride accounts for 1.2 wt%, the ferric nitrate accounts for 5.0%, and the glycol accounts for 0.8%. Performing ultrasonic dispersion for 15min, heating to 215 ℃, reacting for 8h, performing centrifugal separation, washing with absolute ethyl alcohol, performing vacuum drying, and grinding to obtain nano core-shell particles; mixing the modified Chinese juniper oil and the nano core-shell particles, performing ultrasonic dispersion, and performing vacuum drying to obtain an antibacterial agent;
(2) mixing polyethylene resin, an auxiliary agent and an antibacterial agent, and stirring for 50min at the temperature of 67 ℃ to obtain a skin material;
(3) mixing PET resin, an auxiliary agent and an antibacterial agent, and stirring for 50min at the temperature of 90 ℃ to obtain a skin material;
(4) mixing the sheath layer material prepared in the step (2) and the core layer material prepared in the step (3) and adding the mixture into a spinning machine, wherein the mass ratio of the sheath layer material to the core layer material is 3: 2; melting for 50min at 195 deg.C, extruding under high pressure, spraying, water cooling, drafting, oven drying, and cutting to obtain the final product.
Comparative example 1
A medical antibacterial ES fiber is a sheath-core fiber, which is prepared by mixing and spinning a sheath material and a core material; the leather layer material comprises the following raw material components, by weight, 9 parts of leather layer resin, 3 parts of auxiliary agent and 1.5 parts of antibacterial agent; the core layer material comprises the following raw material components, by weight, 9 parts of core layer resin, 3 parts of an auxiliary agent and 1.5 parts of an antibacterial agent.
The antibacterial agent is prepared by mixing the cypress oil and the nano core-shell particles, and the mass ratio of the cypress oil to the nano core-shell particles is 1: 1.
The auxiliary agent comprises 0.7 part of antioxidant, 0.5 part of dispersant, 0.4 part of coupling agent and 0.4 part of antistatic agent.
A preparation process of medical antibacterial ES fiber comprises the following steps;
(1) mixing silver nitrate solution, sodium chloride and ferric nitrate, and adding glycol, wherein the silver nitrate accounts for 1.71 wt%, the sodium chloride accounts for 1.2 wt%, the ferric nitrate accounts for 5.0%, and the glycol accounts for 0.8%. Performing ultrasonic dispersion for 15min, heating to 215 ℃, reacting for 8h, performing centrifugal separation, washing with absolute ethyl alcohol, performing vacuum drying, and grinding to obtain nano core-shell particles; mixing the Chinese juniper oil and the nano core-shell particles, performing ultrasonic dispersion, and performing vacuum drying to obtain an antibacterial agent;
(2) mixing polyethylene resin, an auxiliary agent and an antibacterial agent, and stirring for 50min at the temperature of 67 ℃ to obtain a skin material;
(3) mixing PET resin, an auxiliary agent and an antibacterial agent, and stirring for 50min at the temperature of 90 ℃ to obtain a skin material;
(4) mixing the sheath layer material prepared in the step (2) and the core layer material prepared in the step (3) and adding the mixture into a spinning machine, wherein the mass ratio of the sheath layer material to the core layer material is 3: 2; melting for 50min at 195 deg.C, extruding under high pressure, spraying, water cooling, drafting, oven drying, and cutting to obtain the final product.
Comparative example 2
A medical antibacterial ES fiber is a sheath-core fiber, which is prepared by mixing and spinning a sheath material and a core material; the leather layer material comprises the following raw material components, by weight, 9 parts of leather layer resin, 3 parts of auxiliary agent and 1.5 parts of antibacterial agent; the core layer material comprises the following raw material components, by weight, 9 parts of core layer resin, 3 parts of an auxiliary agent and 1.5 parts of an antibacterial agent.
The antibacterial agent is prepared by mixing modified Chinese juniper oil and nano-silver, and the mass ratio of the modified Chinese juniper oil to the nano-silver is 1: 1.
The auxiliary agent comprises 0.7 part of antioxidant, 0.5 part of dispersant, 0.4 part of coupling agent and 0.4 part of antistatic agent.
A preparation process of medical antibacterial ES fiber comprises the following steps;
(1) adding tetraethyl orthosilicate, ammonium bromide and ammonia water into mesoporous silica, mixing, stirring, heating to 60 ℃, dropwise adding 3-aminopropyltriethoxysilane, stirring, reacting for 7 hours, filtering, washing with an absolute ethanol solution, and drying to obtain a substance A; dissolving polyacrylic acid in hydrochloric acid solution, stirring, adding N-hydroxysuccinimide and the substance A, stirring, filtering to remove solid phase, and drying to obtain a substance B; mixing the Chinese juniper oil with the substance B, ultrasonically dispersing for 30min, filtering, and drying to obtain modified Chinese juniper oil; mixing modified Chinese juniper oil and nano-silver, performing ultrasonic dispersion, and vacuum drying to obtain an antibacterial agent;
(2) mixing polyethylene resin, an auxiliary agent and an antibacterial agent, and stirring for 50min at the temperature of 67 ℃ to obtain a skin layer mixture;
(3) mixing PET resin, an auxiliary agent and an antibacterial agent, and stirring for 50min at the temperature of 90 ℃ to obtain a skin layer mixture;
(4) mixing the skin layer mixture prepared in the step (2) and the core layer mixture prepared in the step (3), and adding the mixture into a spinning machine, wherein the mass ratio of skin layer materials to core layer materials is 3: 2; melting for 50min at 195 deg.C, extruding under high pressure, spraying, water cooling, drafting, oven drying, and cutting to obtain the final product.
Comparative example 3
A medical antibacterial ES fiber is a sheath-core fiber, which is prepared by mixing and spinning a sheath material and a core material; the leather layer material comprises the following raw material components, by weight, 9 parts of leather layer resin, 3 parts of auxiliary agent and 1.5 parts of antibacterial agent; the core layer material comprises the following raw material components, by weight, 9 parts of core layer resin, 3 parts of an auxiliary agent and 1.5 parts of an antibacterial agent.
The antibacterial agent is prepared by mixing Chinese juniper oil and nano-silver, and the mass ratio of the Chinese juniper oil to the nano-silver is 1: 1. The auxiliary agent comprises 0.7 part of antioxidant, 0.5 part of dispersant, 0.4 part of coupling agent and 0.4 part of antistatic agent.
A preparation process of medical antibacterial ES fiber comprises the following steps;
(1) mixing Chinese juniper oil and nano-silver, performing ultrasonic dispersion, and vacuum drying to obtain an antibacterial agent;
(2) mixing polyethylene resin, an auxiliary agent and an antibacterial agent, and stirring for 50min at the temperature of 67 ℃ to obtain a skin material;
(3) mixing PET resin, an auxiliary agent and an antibacterial agent, and stirring for 50min at the temperature of 90 ℃ to obtain a skin material;
(4) mixing the sheath layer material prepared in the step (2) and the core layer material prepared in the step (3) and adding the mixture into a spinning machine, wherein the mass ratio of the sheath layer material to the core layer material is 3: 2; melting for 50min at 195 deg.C, extruding under high pressure, spraying, water cooling, drafting, oven drying, and cutting to obtain the final product.
Comparative example 4
A medical antibacterial ES fiber is a sheath-core fiber, which is prepared by mixing and spinning a sheath material and a core material; the leather layer material comprises the following raw material components, by weight, 9 parts of leather layer resin, 3 parts of auxiliary agent and 1.5 parts of antibacterial agent; the core layer material comprises the following raw material components, by weight, 9 parts of core layer resin, 3 parts of an auxiliary agent and 1.5 parts of an antibacterial agent.
The antibacterial agent is Chinese juniper oil; the auxiliary agent comprises 0.7 part of antioxidant, 0.5 part of dispersant, 0.4 part of coupling agent and 0.4 part of antistatic agent.
A preparation process of medical antibacterial ES fiber comprises the following steps;
(1) mixing polyethylene resin, an auxiliary agent and an antibacterial agent, and stirring for 50min at the temperature of 67 ℃ to obtain a skin material;
(2) mixing PET resin, an auxiliary agent and an antibacterial agent, and stirring for 50min at the temperature of 90 ℃ to obtain a skin material;
(3) mixing the sheath layer material prepared in the step (2) and the core layer material prepared in the step (3) and adding the mixture into a spinning machine, wherein the mass ratio of the sheath layer material to the core layer material is 3: 2; melting for 50min at 195 deg.C, extruding under high pressure, spraying, water cooling, drafting, oven drying, and cutting to obtain the final product.
Comparative example 5
A medical antibacterial ES fiber is a sheath-core fiber, which is prepared by mixing and spinning a sheath material and a core material; the leather layer material comprises the following raw material components, by weight, 9 parts of leather layer resin, 3 parts of auxiliary agent and 1.5 parts of antibacterial agent; the core layer material comprises the following raw material components, by weight, 9 parts of core layer resin, 3 parts of an auxiliary agent and 1.5 parts of an antibacterial agent.
The antibacterial agent is nano silver; the auxiliary agent comprises 0.7 part of antioxidant, 0.5 part of dispersant, 0.4 part of coupling agent and 0.4 part of antistatic agent.
A preparation process of medical antibacterial ES fiber comprises the following steps;
(1) mixing polyethylene resin, an auxiliary agent and an antibacterial agent, and stirring for 50min at the temperature of 67 ℃ to obtain a skin material;
(2) mixing PET resin, an auxiliary agent and an antibacterial agent, and stirring for 50min at the temperature of 90 ℃ to obtain a skin material;
(3) mixing the sheath layer material prepared in the step (2) and the core layer material prepared in the step (3) and adding the mixture into a spinning machine, wherein the mass ratio of the sheath layer material to the core layer material is 3: 2; melting for 50min at 195 deg.C, extruding under high pressure, spraying, water cooling, drafting, oven drying, and cutting to obtain the final product.
Experimental comparison and analysis
In order to more intuitively prove the beneficial effects of the technical scheme of the invention, a comparison experiment is carried out on the technical scheme of the invention and the prior art; the embodiment 1-3 is the technical scheme of the invention;
the antioxidant in the comparative example 1 is prepared by mixing the Chinese juniper oil and the nano core-shell particles, and the rest contents are the same as those in the example 3;
the antioxidant in the comparative example 2 is prepared by mixing modified Chinese juniper oil and nano silver, and the rest contents are the same as those in the example 3;
the antioxidant in the comparative example 3 is the mixture of the Chinese juniper oil and the nano silver, and the rest is the same as the example 3;
comparative example 4 the antioxidant was only juniper oil, and the rest was the same as in example 3;
the antioxidant in comparative example 5 is only nano silver, and the rest is the same as in example 3.
Selecting escherichia coli as a representative of gram-negative bacteria, and selecting staphylococcus aureus as a representative of gram-positive bacteria; according to the regulations of GB/T20944.3-2088 evaluation on antibacterial performance of textiles, the antibacterial rates of the ES fiber samples prepared in examples 1-3 and comparative examples 1-5 on escherichia coli and staphylococcus aureus are detected, and the detection data are shown in the following table 1 in percentage; according to the regulation of GB/T20944.2-2007 part 2 absorption method for evaluating the antibacterial performance of textiles, the antibacterial rate of the ES fiber samples prepared in examples 1-3 and comparative examples 1-5 on fungi is detected, and the monitoring data are shown in the following table 1 in percentage.
| The antibacterial rate of escherichia coli is% | Staphylococcus aureus bacteriostasis rate% | The bacteriostasis rate of the fungus is% | |
| Example 1 | 99.8 | 99.7 | 99.7 |
| Example 2 | 99.8 | 99.8 | 99.9 |
| Example 3 | 99.9 | 99.8 | 99.8 |
| Comparative example 1 | 92.1 | 91.3 | 89.6 |
| Comparative example 2 | 93.5 | 93.0 | 92.7 |
| Comparative example 3 | 90.5 | 90.0 | 89.7 |
| Comparative example 4 | 72.2 | 72.2 | 78.5 |
| Comparative example 5 | 86.0 | 86.4 | 85.2 |
TABLE 1
The breaking strength and breaking elongation of the ES fibers prepared in examples 1 to 3 were measured according to GB/T14337-2008 test method for tensile properties of chemical fiber staple fibers; the test data are shown in table 2 below; the oil content of the chemical fiber is detected according to GB/T6504-2017 chemical fiber oil content test method, the moisture regain is detected according to GB/T6503-2017 chemical fiber moisture regain test method, and the detection data are shown in Table 2
| Example 1 | Example 2 | Example 3 | |
| Breaking strength CN/dtex | 3.22 | 3.25 | 3.39 |
| Elongation at break% | 75.4 | 75.7 | 75.5 |
| The moisture regain percentage is% | 0.15 | 0.13 | 0.13 |
| Oil content% | 0.26 | 0.25 | 0.25 |
TABLE 2
As can be seen from table 1 above, the ES fiber samples prepared in examples 1-3 all have an antibacterial rate of 99.7 or more against escherichia coli, staphylococcus aureus, and fungi, and the antibacterial rate is higher than any one of the groups of comparative examples 1-5, which indicates that the ES fiber prepared by using the modified juniper oil and the nano-core-shell particle mixed antibacterial agent in the technical scheme of the present invention has a higher antibacterial rate than ES fiber prepared by using any one of combination of juniper oil alone, nano-silver alone, mixture of juniper oil and nano-silver, mixture of modified juniper oil and nano-silver, and mixture of juniper oil and nano-core-shell particle, so the technical scheme of the present invention is an optimized scheme, and the prepared ES has a superior antibacterial rate.
As can be seen from the data in Table 2, the ES fibers prepared in examples 1-3 have high breaking strength and elongation at break, and low moisture regain and oil content; the addition of the nano core-shell particles not only improves the antibacterial property, but also enhances the mechanical property of the ES fiber due to the metal characteristic of the nano core-shell particles.
In conclusion, the ES fiber prepared by the invention has strong antibacterial property, good mechanical property, low moisture regain and low oil content.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (9)
1. A medical antibacterial ES fiber is characterized in that: the medical antibacterial ES fiber is a sheath-core fiber and is prepared by mixing and spinning a sheath material and a core material; the leather layer material comprises the following raw material components, by weight, 16-19 parts of leather layer resin, 2-3 parts of auxiliary agent and 0.8-1.5 parts of antibacterial agent; the core layer material comprises the following raw materials, by weight, 16-19 parts of core layer resin, 2-3 parts of an auxiliary agent and 0.8-1.5 parts of an antibacterial agent.
2. The medical antibacterial ES fiber as claimed in claim 1, wherein the antibacterial agent is prepared by mixing modified Chinese juniper oil and nano core-shell particles in a mass ratio of 1-5: 1.
3. The medical antibacterial ES fiber as claimed in claim 2, wherein the modified cypress oil is mainly prepared by reacting cypress oil, mesoporous silica, 3-aminopropyltriethoxysilane, polyacrylic acid; the nano core-shell particles are mainly prepared from silver nitrate and ferric nitrate.
4. The medical antibacterial ES fiber as claimed in claim 1, wherein the sheath resin is a polyethylene resin; the core layer resin is polyethylene terephthalate or polypropylene resin.
5. The medical antibacterial ES fiber according to claim 1, wherein the auxiliary agent comprises 0.7 part of antioxidant, 0.5 part of dispersant, 0.4 part of coupling agent and 0.4 part of antistatic agent.
6. The medical antibacterial ES fiber according to claim 5, wherein the antioxidant is a mixture of a hindered phenol antioxidant and a phosphite antioxidant, the dispersant is succinimide, the coupling agent is any one of stearic acid, calcium stearate and a silane coupling agent, and the antistatic agent is a mixture of glycerol trilaurate and ethoxylated alkyl acid.
7. A preparation process of medical antibacterial ES fiber is characterized by comprising the following steps; (1) preparing an antibacterial agent; (2) preparing a leather material; (3) preparing a core layer material; (4) and mixing and spinning to obtain the medical antibacterial ES fiber.
8. The process for preparing medical antibacterial ES fibers according to claim 7, which comprises the following steps;
(1) adding tetraethyl orthosilicate, ammonium bromide and ammonia water into mesoporous silica, mixing, stirring, heating, dropwise adding 3-aminopropyltriethoxysilane, stirring, reacting, filtering, washing with an absolute ethanol solution, and drying to obtain a substance A; dissolving polyacrylic acid in hydrochloric acid solution, stirring, adding N-hydroxysuccinimide and the substance A, stirring, filtering to remove solid phase, and drying to obtain a substance B; mixing the Chinese juniper oil with the substance B, filtering, and drying to obtain modified Chinese juniper oil;
preparing nano core-shell particles; mixing a silver nitrate solution, sodium chloride and ferric nitrate, adding ethylene glycol, performing ultrasonic dispersion, heating up for reaction, performing centrifugal separation, washing with absolute ethyl alcohol, performing vacuum drying, and grinding to obtain nano core-shell particles; mixing the modified Chinese juniper oil and the nano core-shell particles, performing ultrasonic dispersion, and vacuumizing to remove moisture to obtain an antibacterial agent;
(2) mixing 16-19 parts of polyethylene resin, 2-3 parts of auxiliary agent and 0.8-1.5 parts of antibacterial agent, and stirring at 63-67 ℃ for 40-50min to obtain a skin layer mixture;
(3) mixing 16-19 parts of PET resin, 2-3 parts of auxiliary agent and 0.8-1.5 parts of antibacterial agent, and stirring at 80-90 ℃ for 40-50min to obtain a core layer mixture;
(4) and (3) respectively adding the skin layer mixture prepared in the step (2) and the core layer mixture prepared in the step (3) into a spinning machine, melting, co-extruding, spinning, water cooling, drafting, drying and cutting to prepare the ES fiber.
9. The process for preparing medical antibacterial ES fibers according to claim 8, which comprises the steps of;
(1) adding tetraethyl orthosilicate, ammonium bromide and ammonia water into mesoporous silica, mixing, stirring, heating to 60 ℃, dropwise adding 3-aminopropyltriethoxysilane, stirring, reacting for 6-7h, filtering, washing with an absolute ethanol solution, and drying to obtain a substance A; dissolving polyacrylic acid in hydrochloric acid solution, stirring, adding N-hydroxysuccinimide and the substance A, stirring, filtering to remove solid phase, and drying to obtain a substance B; mixing the Chinese juniper oil with the substance B, ultrasonically dispersing for 20-30min, filtering, and drying to obtain modified Chinese juniper oil;
preparing nano core-shell particles; mixing a silver nitrate solution, sodium chloride and ferric nitrate, adding ethylene glycol, performing ultrasonic dispersion, heating to 205-215 ℃, reacting for 6-8h, performing centrifugal separation, washing with absolute ethyl alcohol, performing vacuum drying, and grinding to obtain nano core-shell particles;
mixing the modified Chinese juniper oil and the nano core-shell particles, performing ultrasonic dispersion, and performing vacuum drying to remove moisture to obtain an antibacterial agent;
(2) mixing 16-19 parts of polyethylene resin, 2-3 parts of auxiliary agent and 0.8-1.5 parts of antibacterial agent, and stirring at 63-67 ℃ for 40-50min to obtain a skin layer mixture;
(3) mixing 16-19 parts of PET resin, 2-3 parts of auxiliary agent and 0.8-1.5 parts of antibacterial agent, and stirring at 80-90 ℃ for 40-50min to obtain a core layer mixture;
(4) respectively adding the skin layer mixture prepared in the step (2) and the core layer mixture prepared in the step (3) into a spinning machine, wherein the mass ratio of skin layer materials to core layer materials is 3: 2; melting for 40-50min at the temperature of 185-195 ℃, co-extruding, spinning, water-cooling, drafting, drying and cutting to obtain the medical antibacterial ES fiber finished product.
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| CN112430867A (en) * | 2020-11-18 | 2021-03-02 | 广州唐斯科技有限公司 | ES fiber containing porous molecular nest and preparation method and application thereof |
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| CN116555933B (en) * | 2023-05-31 | 2024-02-02 | 芝诺(苏州)生物科技有限公司 | ES macrobiological fiber containing 2' -fucosyllactose and seaweed extract and preparation method thereof |
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