CN110699955A - Production process of polylactic acid functional non-woven fabric - Google Patents

Production process of polylactic acid functional non-woven fabric Download PDF

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CN110699955A
CN110699955A CN201910811531.1A CN201910811531A CN110699955A CN 110699955 A CN110699955 A CN 110699955A CN 201910811531 A CN201910811531 A CN 201910811531A CN 110699955 A CN110699955 A CN 110699955A
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polylactic acid
woven fabric
reaction
production process
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董纹吉
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Kunshan Jiehong Nonwoven Products Co Ltd
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03Polysaccharides or derivatives thereof
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    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/06Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from hydroxycarboxylic acids
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    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/91Polymers modified by chemical after-treatment
    • C08G63/912Polymers modified by chemical after-treatment derived from hydroxycarboxylic acids
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/78Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
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    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/07Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/11Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
    • D06M11/28Halides of elements of Groups 8, 9, 10 or 18 of the Periodic Table
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    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/51Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/55Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
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    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
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    • D06M16/00Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract

A production process of polylactic acid functional non-woven fabric comprises the following steps: modifying polylactic acid, preparing polylactic acid fibers, preparing polylactic acid non-woven fabrics, and preparing polylactic acid functional non-woven fabrics, wherein the modification of the polylactic acid comprises the steps of carrying out rotary evaporation on industrial L lactic acid to obtain refined lactic acid, putting the refined lactic acid into a reaction kettle, adding a catalyst and reactive montmorillonite, obtaining a reactant after the reaction is finished, purifying the reactant, and drying to obtain the modified polylactic acid. The production process of the polylactic acid functional non-woven fabric is prepared from the modified polylactic acid, is completely degraded under natural conditions, is harmless to the environment, has improved mechanical properties and good hydrophilicity and adhesiveness, comprehensively utilizes the film forming bacteriostasis of chitosan and the natural oxidation resistance of tea polyphenol, has good antibacterial effect, is free from the influence of various microorganisms and environmental factors, and has long shelf life and wide application prospect.

Description

Production process of polylactic acid functional non-woven fabric
Technical Field
The invention belongs to the technical field of non-woven fabrics, and particularly relates to a production process of a polylactic acid functional non-woven fabric.
Background
Environmental protection problems are very important in all countries around the world, relevant policies and regulations are developed to support biomass plastics, and from 2008 to 1 month in China, plastic shopping bags with the thickness of less than 0.025 mm are prohibited to be produced, sold and used nationwide, and the medical field is the market for polylactic acid to enter at the earliest.
Polylactic acid is a polymer obtained by polymerizing lactic acid as a main raw material, and the raw material is sufficiently available and can be regenerated. The production process of polylactic acid is pollution-free, and the product can be biodegraded, thus realizing the circulation in nature, and being an ideal green high polymer material. The polylactic acid has unique biocompatibility and biodegradability compared with other common polymer materials, is approved by the Food and Drug Administration (FDA) of the United states and can be used for human bodies, such as producing disposable transfusion tools, non-dismantling surgical sutures, orthopedic fixing pieces, bone nails, surgical devices, medical stents, biological catheters and the like, and the low molecular weight polylactic acid can be used as a slow-release drug wrapping material.
The 'twelve five new material industry' program published by the national development committee in 2012 provides a positive development on the research of biodegradable materials such as polylactic acid and the like, and accelerates the realization of industrialization and the promotion of the industrial development of bio-based high polymer materials and bio-based green chemicals. The ' twelve-five ' program for development of bio-industry ' published in 2013 clearly indicates that non-grain raw material production of a batch of important bio-based products is realized, and the development and application of technologies such as chemical polymerization of bio-based materials are promoted.
Because polylactic acid is a semi-crystalline polymer, has low crystallization rate, high hardness, poor processing thermal stability, narrow processing temperature window and the like, the application of polylactic acid in the field of non-woven fabrics is limited to a certain extent, and the modification of polylactic acid is a hotspot of research. The development of polylactic acid functional non-woven fabrics can promote the development of the non-woven fabric industry and related industries, promote the independent innovation capability of the related industries, and have good market prospect.
Chinese patent application No. CN201810772945.3 discloses a medical magnetic therapy elastic non-woven fabric with high water absorption and high air permeability, which comprises the following components: 20-27 parts of modified polylactic acid fiber, 20-33 parts of modified bamboo fiber, 10-20 parts of hydroxymethyl cellulose, 2-5 parts of casein, 20-30 parts of soybean protein fiber, 5-10 parts of sodium alginate, 20-35 parts of starch, 20-23 parts of magnetic starch, 40-45 parts of modified polyacrylamide fiber and 3-5 parts of plant extract, and the fiber material is a magnetic therapy functional fiber material.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects, the invention aims to provide a production process of polylactic acid functional non-woven fabric, which is prepared from modified polylactic acid, aiming at the defects of low strength, poor toughness and the like of the polylactic acid, reactive montmorillonite is added into the polylactic acid, and the reactive montmorillonite reacts with terminal carboxyl on a polylactic acid molecular chain segment to prepare the modified polylactic acid, so that the purpose of effectively improving the defects of the polylactic acid is achieved. Compared with pure polylactic acid, the formed modified polylactic acid has better comprehensive performance, improved impact modulus, improved elongation at break, improved strength and improved thermal stability. The polylactic acid functional non-woven fabric can be completely degraded under natural conditions, is harmless to the environment, safe and environment-friendly, has good mechanical property, hydrophilicity and adhesiveness, comprehensively utilizes the film forming bacteriostasis of chitosan and the natural oxidation resistance of tea polyphenol, has good antibacterial effect, is free from the influence of various microorganisms and environmental factors, and has long quality guarantee period and wide application prospect.
The purpose of the invention is realized by the following technical scheme:
a production process for polylactic acid functional non-woven fabric is characterized by comprising the following steps:
(1) modification of polylactic acid: carrying out rotary evaporation on industrial L lactic acid to obtain refined lactic acid, putting the refined lactic acid into a reaction kettle, adding a catalyst and reactive montmorillonite, obtaining a reactant after the reaction is finished, purifying the reactant, and drying to obtain modified polylactic acid;
(2) preparation of polylactic acid fiber: the modified polylactic acid is prepared by a melt blowing method, polylactic acid melt is blown into polylactic acid fibers through spinneret orifices, the temperature of the polylactic acid melt is 180 ℃, the size of the spinneret orifices is 0.5mm, and the speed of the spinneret orifices is 600 m/min;
(3) preparing polylactic acid non-woven fabric: carrying out air flow drawing on the polylactic acid fiber to form a reticular fiber with filaments uniformly laid, and carrying out hot roller bonding on the reticular fiber to obtain a polylactic acid non-woven fabric;
(4) preparation of polylactic acid functional non-woven fabric: and (2) carrying out surface hydrophilic modification on the polylactic acid non-woven fabric, soaking the modified polylactic acid non-woven fabric in a chitosan/tea polyphenol mixed solution, putting the mixture into a constant temperature and humidity box for 24 hours, taking out and drying the mixture, wherein the drying temperature is 60 ℃, and thus obtaining the polylactic acid functional non-woven fabric.
Aiming at the defects of low strength, poor toughness and the like of the polylactic acid, the reactive montmorillonite is added into the polylactic acid, and the reactive montmorillonite reacts with terminal carboxyl on a polylactic acid molecular chain segment to prepare the modified polylactic acid so as to achieve the aim of effectively improving the defects of the polylactic acid. Compared with pure polylactic acid, the formed modified polylactic acid has better comprehensive performance, improved impact modulus, elongation at break, strength and thermal stability, and can realize the aim of environment-friendly sustainable development in the fields of food packaging, disposable products, medical health and the like.
The polylactic acid non-woven fabric is a high-crystalline material, has no polar groups on the surface, shows hydrophobicity, and is not easy to compound with hydrophilic active substances such as chitosan and tea polyphenol. It is required to increase the hydrophilicity and adhesion of the polylactic acid nonwoven fabric by hydrophilic modification of the surface thereof while maintaining mechanical properties such as high tensile force and tensile strength.
Chitosan is a representative of natural bacteriostatic agents, but because the chitosan has extremely weak antioxidant activity and only has inhibitory action on a small part of microorganisms, namely the chitosan has narrow bacteriostatic spectrum, and has the defects of low strength, high brittleness and the like, the chitosan application range is limited, and the tea polyphenol has extremely strong oxidation resistance and corrosion resistance, and is a natural bacteriostatic agent, the polylactic acid functional non-woven fabric disclosed by the invention uses the chitosan as a bacteriostatic film-forming agent and the tea polyphenol as an antioxidant, the surface hydrophilic modification of the polylactic acid non-woven fabric is firstly improved to increase the hydrophilicity and the adhesiveness of the polylactic acid non-woven fabric, then the polylactic acid functional non-woven fabric is prepared in a dip coating mode, and the natural bioactive agents of chitosan and tea polyphenol are combined with the modified polylactic acid non-woven fabric by using a chitosan/tea polyphenol compound mixed solution, so that the film-forming bacteriostatic action of the chitosan is comprehensively utilized, The polylactic acid functional non-woven fabric has the advantages of good antibacterial effect, no influence of various microorganisms and environmental factors, long quality guarantee period, good mechanical property, complete degradation under natural conditions, generation of carbon dioxide and water which are harmless to the environment, no pollution, expansion of the application field of the non-woven fabric, suitability for industrial production, environmental friendliness and no pollution.
Further, in the production process for the polylactic acid functional non-woven fabric, the catalyst is a composite catalyst of p-toluenesulfonic acid and stannous chloride, and the molar ratio of the p-toluenesulfonic acid to the stannous chloride is 1: 1.
Further, in the production process for the polylactic acid functional non-woven fabric, the preparation method of the reactive montmorillonite comprises the following steps:
(1) activating organic montmorillonite with polyphosphoric acid in advance;
(2) and adding the treated organic montmorillonite into an ethanol solution of dopamine, reacting for 60min, filtering, and drying to obtain the reactive montmorillonite.
The organic montmorillonite is activated in advance by polyphosphoric acid, so that the original interlayer binding force is weakened, the interlayer lattice is cracked, and the interlayer spacing is enlarged, thereby being beneficial to the reaction of polyphosphoric acid and dopamine between layers. The dispersion condition and compatibility of the reactive montmorillonite in the polylactic acid matrix can be enhanced by adding the treated organic montmorillonite into an ethanol solution of dopamine.
Further, the production process for the polylactic acid functional non-woven fabric is characterized in that the mass concentration of the dopamine ethanol solution is 20%, and the weight ratio of the organic montmorillonite to the polyphosphoric acid to the dopamine is 40: 20: 25.
further, the production process for the polylactic acid functional non-woven fabric comprises the following steps:
(1) sodium-based montmorillonite is taken out and put in deionized water, and mechanical stirring is carried out for 1 hour at room temperature, so that the sodium-based montmorillonite is fully swelled, and uniform suspension is formed;
(2) heating the suspension to 70 ℃, and adding a dilute hydrochloric acid solution until the pH value of the suspension is 6;
(3) adding a surfactant and isopropanol to prepare an aqueous solution, adding the aqueous solution into the suspension, continuously stirring for 30min, and continuously reacting for 30 min;
(4) after the reaction is finished, putting the reaction solution into ultrasonic waves at the temperature of 80 ℃, and continuing the ultrasonic reaction for 15 min;
(5) and (3) standing, cooling, performing suction filtration and washing after the ultrasound is finished, drying the filtered substance in a vacuum drying oven at 45 ℃ to constant weight, grinding, and sieving with a 200-mesh sieve to obtain the organic montmorillonite clay.
The addition amount of the surfactant and the isopropanol is 1.1 times of the theoretical ion exchange capacity of the sodium-based montmorillonite. By adding the surfactant and the isopropanol, the organic chain segments are vertically arranged between the sodium montmorillonite layers, so that the interlayer spacing of the organic montmorillonite can be effectively increased, and the ion exchange reaction can be fully performed. The hydroxyl on the interlaminar organic chain of the organic montmorillonite reacts with the end carboxyl of the polylactic acid, so that the performance modification effect of the reactive montmorillonite on the polylactic acid is improved.
Further, in the above production process for polylactic acid functional non-woven fabric, the reaction conditions of step (1) include: the initial reaction temperature is 120 ℃, the vacuum degree is 0.07MPa, the reaction is carried out for 4 hours under the protection of N2, then the temperature is raised to 145 ℃, the vacuum degree is 0.1MPa, the reaction is carried out for 2 hours under the protection of N2, finally the temperature is raised to 180 ℃, the vacuum degree is 0.1MPa, and the reaction is carried out for 10 hours under the protection of N2.
Further, in the above production process for polylactic acid functional non-woven fabric, the surface hydrophilic modification in the step (5) includes the following steps:
(1) pretreatment: soaking the polylactic acid non-woven fabric in absolute ethyl alcohol for 24 hours, repeatedly cleaning the polylactic acid non-woven fabric with distilled water, drying the polylactic acid non-woven fabric at 65 ℃, and taking the polylactic acid non-woven fabric out for later use;
(2) surface hydrophilic modification treatment: soaking the pretreated polylactic acid non-woven fabric in corrosive liquid prepared from concentrated sulfuric acid and ferric chloride, placing the soaked polylactic acid non-woven fabric in a water bath kettle at 35 ℃ for reacting for 4 hours, drying, then soaking in distilled water for 8 hours, drying and then taking out to obtain the modified polylactic acid non-woven fabric.
The polylactic acid non-woven fabric is subjected to hydrophilic modification by using the acidic oxidation corrosive liquid formed by concentrated sulfuric acid and ferric chloride, and the method has the advantages of simple process, easiness in operation, low cost and easiness in realization of industrial production.
Further, in the above production process for polylactic acid functional non-woven fabric, the corrosive liquid prepared from concentrated sulfuric acid and ferric chloride is prepared by adding 270g of FeCl3 & 6H2O to 1L of concentrated sulfuric acid with the mass fraction of 15% and completely dissolving.
Further, the preparation method of the chitosan/tea polyphenol mixed solution for the production process of the polylactic acid functional non-woven fabric comprises the following steps:
(1) dissolving chitosan in 1% acetic acid solution, and mechanically dispersing to obtain 1.5% chitosan solution;
(2) and adding tea polyphenol into the chitosan solution every 30 minutes for four times, and dispersing and stirring for 2 hours to obtain the chitosan/tea polyphenol mixed solution.
Further, in the production process for the polylactic acid functional non-woven fabric, the mass ratio of the chitosan to the tea polyphenol in the chitosan/tea polyphenol mixed solution is 1: 1.
compared with the prior art, the invention has the following beneficial effects:
(1) aiming at the defects of low strength, poor toughness and the like of polylactic acid, the production process of the polylactic acid functional non-woven fabric adds reactive montmorillonite into the polylactic acid, and enables the reactive montmorillonite to react with terminal carboxyl on a polylactic acid molecular chain segment to prepare the modified polylactic acid so as to achieve the aim of effectively improving the defects of the polylactic acid, compared with pure polylactic acid, the formed modified polylactic acid has better comprehensive performance, improved impact modulus, improved elongation at break, improved strength and improved thermal stability, and can realize the aim of environment-friendly sustainable development in the fields of food packaging, disposable products, medical sanitation and the like;
(2) according to the production process of the polylactic acid functional non-woven fabric, the acidic oxidation corrosive liquid formed by concentrated sulfuric acid and ferric chloride is adopted to carry out hydrophilic modification on the polylactic acid non-woven fabric, so that the hydrophilicity and the adhesion of the polylactic acid functional non-woven fabric are increased, and the high mechanical properties such as tensile force and tensile strength of the polylactic acid functional non-woven fabric are maintained;
(3) the production process for the polylactic acid functional non-woven fabric combines natural biological active agents of chitosan and tea polyphenol with the modified polylactic acid non-woven fabric, comprehensively utilizes the film forming bacteriostasis of the chitosan, the natural oxidation resistance of the tea polyphenol and the high mechanical property of the polylactic acid non-woven fabric to obtain the polylactic acid functional non-woven fabric, has good antibacterial effect, long shelf life and good mechanical property, is free from the influence of various microorganisms and environmental factors, can be completely degraded under natural conditions to generate carbon dioxide and water which are harmless to the environment, cannot cause pollution, expands the application field of the non-woven fabric, is suitable for industrial production, is environment-friendly and nuisanceless.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to specific experimental data, 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.
The following embodiment provides a production process of a polylactic acid functional non-woven fabric, wherein the catalyst is a composite catalyst of p-toluenesulfonic acid and stannous chloride, and the molar ratio of the p-toluenesulfonic acid to the stannous chloride is 1: 1.
Further, the mass concentration of the dopamine ethanol solution is 20%, and the weight ratio of the organic montmorillonite, the polyphosphoric acid and the dopamine is 40: 20: 25.
the etching solution prepared from concentrated sulfuric acid and ferric chloride is prepared by adding 270g FeCl3 & 6H2O into 1L of concentrated sulfuric acid with the mass fraction of 15% and completely dissolving.
Further, the mass ratio of chitosan to tea polyphenol in the chitosan/tea polyphenol mixed solution is 1: 1.
examples
Preparing organic montmorillonite:
(1) sodium-based montmorillonite is taken out and put in deionized water, and mechanical stirring is carried out for 1 hour at room temperature, so that the sodium-based montmorillonite is fully swelled, and uniform suspension is formed;
(2) heating the suspension to 70 ℃, and adding a dilute hydrochloric acid solution until the pH value of the suspension is 6;
(3) adding a surfactant and isopropanol to prepare an aqueous solution, adding the aqueous solution into the suspension, continuously stirring for 30min, and continuously reacting for 30 min;
(4) after the reaction is finished, putting the reaction solution into ultrasonic waves at 80 ℃, and continuing the ultrasonic reaction for 15 min;
(5) and (3) standing, cooling, performing suction filtration and washing after the ultrasonic treatment is finished, drying the filtered substance in a vacuum drying oven at 45 ℃ to constant weight, grinding, and sieving with a 200-mesh sieve to obtain the organic montmorillonite clay.
Preparation of reactive montmorillonite:
(1) activating organic montmorillonite with polyphosphoric acid in advance;
(2) and adding the treated organic montmorillonite into an ethanol solution of dopamine, reacting for 60min, filtering, and drying to obtain the reactive montmorillonite.
Modification of polylactic acid: carrying out rotary evaporation on industrial L lactic acid to obtain refined lactic acid, putting the refined lactic acid into a reaction kettle, adding a catalyst and reactive montmorillonite, carrying out reaction for 4 hours under the protection of N2 at an initial reaction temperature of 120 ℃ and a vacuum degree of 0.07MPa, then heating to 145 ℃ and a vacuum degree of 0.1MPa under the protection of N2 for 2 hours, finally heating to 180 ℃ and a vacuum degree of 0.1MPa under the protection of N2, reacting for 10 hours to obtain a reactant after the reaction is finished, purifying the reactant, and drying to obtain modified polylactic acid.
Preparation of polylactic acid fiber: the modified polylactic acid is prepared by a melt-blowing method, polylactic acid melt is blown into polylactic acid fibers through spinneret orifices, the temperature of the polylactic acid melt is 180 ℃, the size of the spinneret orifices is 0.5mm, and the speed of the spinneret orifices is 600 m/min.
Preparing polylactic acid non-woven fabric: and carrying out air flow drawing on the polylactic acid fiber to form a reticular fiber with uniformly laid filaments, and carrying out hot roller bonding on the reticular fiber to obtain the polylactic acid non-woven fabric.
Preparation of polylactic acid functional non-woven fabric: and after carrying out surface hydrophilic modification on the polylactic acid non-woven fabric, soaking the modified polylactic acid non-woven fabric in a chitosan/tea polyphenol mixed solution, putting the mixture into a constant temperature and humidity box for 24 hours, taking out and drying the mixture, wherein the drying temperature is 60 ℃, and thus obtaining the polylactic acid functional non-woven fabric.
Effect verification:
according to the production process for the polylactic acid functional non-woven fabric, the polylactic acid functional non-woven fabric of the embodiment is obtained. The samples (1) of the polylactic acid functional nonwoven fabric of the examples and the common polylactic acid nonwoven fabric (2) on the market were subjected to the comparison of the antibacterial property test, the mechanical test and the water contact angle test. The test data are shown in table 1.
TABLE 1
Figure BDA0002185186110000111
(1) And (3) testing antibacterial performance: staphylococcus aureus and Escherichia coli are selected as experimental strains, and according to the national standard GB/120944.1-2007 evaluation part 1 of antibacterial performance of textiles: the agar plate diffusion method tests the antibacterial performance of a sample (1) of the polylactic acid functional non-woven fabric of the embodiment and a common polylactic acid non-woven fabric (2) on the market, uses a vernier caliper to measure the diameter of a bacteriostatic ring around the fabric sample, all the test samples are prepared into round pieces with the diameter of 8mm, the antibacterial effect is evaluated according to the width of the bacteriostatic zone and the propagation condition of bacteria under the sample, and the calculation of the width of the bacteriostatic zone is shown as the formula (1).
D=(d1-d0)/2
In the formula, D is the width of the bacteriostatic band; d1 and d0 are the outer diameter of the zone and the diameter of the test specimen, respectively.
(2) And (3) mechanical testing: according to GB/13923.1-2013, mechanical properties of a sample (1) of the polylactic acid functional non-woven fabric in the embodiment and a common polylactic acid non-woven fabric (2) in the market are tested by an electronic tensile tester, data such as tensile index, elongation at break, tensile strength and the like of each sample are recorded, and the average value is taken after each sample is tested for 3 times.
(3) Water contact angle test: the samples (1) of the polylactic acid functional nonwoven fabric of the examples and the commercially available ordinary polylactic acid nonwoven fabric (2) were subjected to hydrophilicity/hydrophobicity test using a DSA100 type contact angle measuring instrument. Before the test, the sample is cut into a proper size and fixed on a glass slide, the glass slide is placed on a sample table, the volume of water drops is set to be 2 mu L by a pendant drop method for testing, the angle of a contact angle is recorded, and an average value is obtained by measuring 2 times in each group.
As can be seen from table 1, the polylactic acid functional nonwoven fabric of the above embodiment obtained by the production process for polylactic acid functional nonwoven fabric has better antibacterial property, better mechanical property and obvious hydrophilic modification effect compared with the nonwoven fabric on the market.
The invention has many applications, and the above description is only a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention, and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that various modifications can be made without departing from the spirit of the invention, and such modifications are to be considered within the scope of the invention.

Claims (10)

1. A production process of polylactic acid functional non-woven fabric is characterized by comprising the following steps:
(1) modification of polylactic acid: carrying out rotary evaporation on industrial L lactic acid to obtain refined lactic acid, putting the refined lactic acid into a reaction kettle, adding a catalyst and reactive montmorillonite, obtaining a reactant after the reaction is finished, purifying the reactant, and drying to obtain modified polylactic acid;
(2) preparation of polylactic acid fiber: the modified polylactic acid is prepared by a melt blowing method, polylactic acid melt is blown into polylactic acid fibers through spinneret orifices, the temperature of the polylactic acid melt is 180 ℃, the size of the spinneret orifices is 0.5mm, and the speed of the spinneret orifices is 600 m/min;
(3) preparing polylactic acid non-woven fabric: carrying out air flow drawing on the polylactic acid fiber to form a reticular fiber with uniformly laid filaments, and carrying out hot roller bonding on the reticular fiber to obtain a polylactic acid non-woven fabric;
(4) preparation of polylactic acid functional non-woven fabric: and after carrying out surface hydrophilic modification on the polylactic acid non-woven fabric, soaking the modified polylactic acid non-woven fabric in a chitosan/tea polyphenol mixed solution, putting the mixture into a constant temperature and humidity box for 24 hours, taking out and drying the mixture, wherein the drying temperature is 60 ℃, and thus obtaining the polylactic acid functional non-woven fabric.
2. The production process of the polylactic acid functional non-woven fabric according to claim 1, wherein the catalyst is a composite catalyst of p-toluenesulfonic acid and stannous chloride, and the molar ratio of the p-toluenesulfonic acid to the stannous chloride is 1: 1.
3. The production process of the polylactic acid functional non-woven fabric according to claim 1, wherein the preparation method of the reactive montmorillonite comprises the following steps:
(1) activating organic montmorillonite with polyphosphoric acid in advance;
(2) and adding the treated organic montmorillonite into an ethanol solution of dopamine, reacting for 60min, filtering, and drying to obtain the reactive montmorillonite.
4. The production process of the polylactic acid functional non-woven fabric according to claim 3, wherein the mass concentration of the dopamine ethanol solution is 20%, and the weight ratio of the organic montmorillonite, the polyphosphoric acid and the dopamine is 40: 20: 25.
5. the production process of the polylactic acid functional non-woven fabric according to claim 3, wherein the preparation method of the organic montmorillonite comprises the following steps:
(1) adding sodium-based montmorillonite into deionized water, mechanically stirring at room temperature for 1h to fully swell the sodium-based montmorillonite and form uniform suspension;
(2) heating the suspension to 70 ℃, and adding a dilute hydrochloric acid solution until the pH value of the suspension is 6;
(3) adding a surfactant and isopropanol to prepare an aqueous solution, adding the aqueous solution into the suspension, continuously stirring for 30min, and continuously reacting for 30 min;
(4) after the reaction is finished, putting the reaction solution into ultrasonic waves at the temperature of 80 ℃, and continuing the ultrasonic reaction for 15 min;
(5) and (3) standing, cooling, performing suction filtration and washing after the ultrasonic treatment is finished, drying the filtered substance in a vacuum drying oven at 45 ℃ to constant weight, grinding, and sieving with a 200-mesh sieve to obtain the organic montmorillonite.
6. The process for producing a polylactic acid functional non-woven fabric according to claim 1, wherein the reaction conditions of the step (1) comprise: the initial reaction temperature is 120 ℃, the vacuum degree is 0.07MPa, the reaction is carried out for 4 hours under the protection of N2, then the temperature is increased to 145 ℃, the vacuum degree is 0.1MPa, the reaction is carried out for 2 hours under the protection of N2, finally the temperature is increased to 180 ℃, the vacuum degree is 0.1MPa, and the reaction is carried out for 10 hours under the protection of N2.
7. The process for producing polylactic acid functional non-woven fabric according to claim 1, wherein the surface hydrophilic modification in the step (5) comprises the steps of:
(1) pretreatment: soaking the polylactic acid non-woven fabric in absolute ethyl alcohol for 24 hours, repeatedly cleaning the polylactic acid non-woven fabric with distilled water, drying the polylactic acid non-woven fabric at 65 ℃, and taking the polylactic acid non-woven fabric out for later use;
(2) surface hydrophilic modification treatment: soaking the pretreated polylactic acid non-woven fabric in corrosive liquid prepared from concentrated sulfuric acid and ferric chloride, placing the non-woven fabric in a water bath kettle at 35 ℃ for reacting for 4 hours, drying, soaking in distilled water for 8 hours, drying and taking out to obtain the modified polylactic acid non-woven fabric.
8. The process for producing a polylactic acid functional nonwoven fabric according to claim 6, wherein the etching solution prepared from concentrated sulfuric acid and ferric chloride is prepared by adding 270g of FeCl 3-6H 2O to 1L of concentrated sulfuric acid with a mass fraction of 15% and completely dissolving the solution.
9. The production process of the polylactic acid functional non-woven fabric according to claim 1, wherein the preparation method of the chitosan/tea polyphenol mixed solution comprises the following steps:
(1) dissolving chitosan in 1% acetic acid solution, and mechanically dispersing to obtain 1.5% chitosan solution;
(2) and adding tea polyphenol into the chitosan solution every 30 minutes for four times, and dispersing and stirring for 2 hours to obtain the chitosan/tea polyphenol mixed solution.
10. The production process of the polylactic acid functional non-woven fabric according to claim 8, wherein the mass ratio of the chitosan to the tea polyphenol in the chitosan/tea polyphenol mixed solution is 1: 1.
CN201910811531.1A 2019-08-30 2019-08-30 Production process of polylactic acid functional non-woven fabric Pending CN110699955A (en)

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CN111893751A (en) * 2020-07-23 2020-11-06 杭州众逸布业有限公司 Fireproof bacteriostatic curtain fabric and preparation method thereof
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CN112391739A (en) * 2020-12-01 2021-02-23 金晓红 Polylactic acid ecological antibacterial fiber underwear and production process thereof
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US12012681B2 (en) 2021-06-28 2024-06-18 China Yunhong Holdings Co., Ltd. Method for preparing fully-degradable non-woven fabric by spun-bonding
CN113862903A (en) * 2021-12-01 2021-12-31 北京石墨烯技术研究院有限公司 Modified polylactic acid non-woven fabric and preparation method and application thereof
CN113862903B (en) * 2021-12-01 2022-02-22 北京石墨烯技术研究院有限公司 Modified polylactic acid non-woven fabric and preparation method and application thereof
CN114369906A (en) * 2021-12-30 2022-04-19 广东宝创环保新材料制品有限公司 Environment-friendly easily-degradable antibacterial non-woven fabric and preparation method thereof
CN114369906B (en) * 2021-12-30 2023-09-08 广东宝创环保新材料制品有限公司 Environment-friendly and easily-decomposed antibacterial non-woven fabric and preparation method thereof
CN115624646A (en) * 2022-10-25 2023-01-20 维达纸业(浙江)有限公司 Antibacterial liquid-absorbing non-woven material for hygienic products
CN115624646B (en) * 2022-10-25 2023-09-05 维达纸业(浙江)有限公司 Antibacterial liquid-absorbing nonwoven material for sanitary products

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