CN114044834B - Polylactic acid fiber and application thereof in adult incontinence nursing pad - Google Patents
Polylactic acid fiber and application thereof in adult incontinence nursing pad Download PDFInfo
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- CN114044834B CN114044834B CN202111286883.3A CN202111286883A CN114044834B CN 114044834 B CN114044834 B CN 114044834B CN 202111286883 A CN202111286883 A CN 202111286883A CN 114044834 B CN114044834 B CN 114044834B
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- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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Abstract
The invention discloses a polylactic acid fiber and application thereof in adult incontinence nursing pads, belonging to the technical field of sanitary materials, and specifically comprising the following components in parts by weight: firstly, the dibenzoyl tartaric acid and the 4- (2, 3-epoxypropoxy) indole are utilized to modify chitosan to obtain a chitosan derivative, then the chitosan is utilized to carry out blending modification on polylactic acid to obtain polylactic acid fiber, and finally, the polylactic acid fiber is prepared into a non-woven fabric material through mixing, opening, cotton feeding, carding, direct web formation and hot rolling reinforcement.
Description
Technical Field
The invention belongs to the technical field of sanitary materials, and particularly relates to polylactic acid fiber and application thereof in an adult incontinence nursing pad.
Background
In recent years, the aging degree of the Chinese population is increased continuously, the population of the aged people over 16 percent of the total population in 60 years old and older in China provides huge potential consumer groups for the market of adult incontinence products in China, so that the consumption of adult incontinence nursing pads is increased year by year, and the adult incontinence nursing pads are disposable sanitary products which are discarded after being used, so that the consumption of the adult incontinence nursing pads is huge every year. The problem of product disposal is behind huge consumption, and the adult incontinence nursing pad occupies a lot of precious resources due to volume expansion after absorbing water, and the environment pollution is caused by burning, so that the development of the degradable adult incontinence nursing pad is very important for reducing the pollution and waste of the environment resources.
The polylactic acid fiber is a novel ecological environment-friendly fiber, which is a synthetic polyester prepared by taking corn starch as a raw material and carrying out a series of reactions such as fermentation, condensation, polymerization and the like. The polylactic acid has the advantages of wide source of raw materials, regeneration, complete biodegradation, high transparency, good oil resistance and dyeing property, low flammability, no toxicity to human bodies and the like, and can be used for various forming processing, such as extrusion, film blowing, injection molding, fiber forming and the like. Therefore, the polylactic acid has wide application prospect in adult incontinence nursing pads. Although polylactic acid has the above advantages, the crystallization rate of polylactic acid is very slow, the melt strength is low, and the molding process is difficult; the glass transition temperature is low, and the heat resistance is poor; the melt is easy to degrade in the processing process, and the molecular weight distribution are difficult to control; the product is brittle and hard, has poor toughness, lacks flexibility and elasticity, and has small impact strength. These disadvantages severely limit the application of polylactic acid materials. The prior art discloses that polylactic acid fibers are used for preparing adult incontinence nursing pads, for example, patent 201210576102.9 discloses a completely degradable non-woven fabric material, specifically, polylactic acid bi-component fibers and polylactic acid fibers are mixed, loosened and carded, and then are penetrated by hot air and are subjected to hot rolling reinforcement to prepare the completely degradable non-woven material, so that the completely degradable non-woven fabric material has the advantages of good strength, difficulty in fiber falling, high permeation moisture conduction speed, complete degradation and the like, is an ideal material for preparing adult incontinence nursing pads, and is still not ideal in strength, toughness, air permeability and the like. In order to make up for the defects of polylactic acid materials and make the polylactic acid materials better applicable to the field of sanitary materials such as adult incontinence nursing pads, further modification is needed.
Disclosure of Invention
The invention provides polylactic acid fiber for overcoming the defects in the prior art, and the polylactic acid fiber is prepared into a non-woven fabric material to be used as the surface layer of the adult incontinence nursing pad, has the advantages of high strength, good toughness, high moisture permeability, soft hand feeling, fluffiness and air permeability, has high degradation rate, and reduces the pollution to the environment.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for preparing chitosan derivatives comprises the following steps:
s1, reacting dibenzoyl tartaric acid with amino in chitosan to obtain N-carboxyl acylation chitosan;
s2, 4- (2, 3-epoxy propoxy) indole reacts with hydroxyl in the N-carboxylic acylation chitosan to obtain the chitosan derivative.
Further, the specific operation steps of step S1 are:
adding chitosan into dimethylformamide, stirring, adding dibenzoyltartaric acid and water reducing agent, introducing N 2 Protecting, stirring and reacting for 3-24h at 100-150 ℃ and 600-1500r/min, adding acetone for precipitation, washing with alcohol and ether for several times, and drying to obtain the N-carboxylic acylated chitosan.
Further, the weight average molecular weight of the chitosan is 3 to 10 ten thousand, preferably 5 to 8 ten thousand; the degree of deacetylation is greater than or equal to 85%, preferably greater than or equal to 90%.
Further, the addition amount of the chitosan is 1-5% of the mass of the dimethylformamide.
Furthermore, the dibenzoyl tartaric acid is added in an amount of 120-200% by mass of the chitosan.
Furthermore, the water reducing agent is 1-ethyl-3 (3-dimethylaminopropyl) carbodiimide hydrochloride, and the addition amount of the water reducing agent is 80-150% of the mass of the chitosan.
Further, the specific operation steps of step S2 are:
adding N-carboxylic acylated chitosan into dimethylformamide, adding a catalyst, stirring and reacting at 40-50 ℃ and 600-1000r/min for 20-50min, then heating to 50-60 ℃, adding 4- (2, 3-epoxypropoxy) indole, continuously stirring for 4-8h, after the reaction is finished, carrying out rotary evaporation to remove organic micromolecules and water, washing with acetone for several times, and drying to obtain the chitosan derivative.
Further, the N-carboxyacylated chitosan is added in an amount of 0.5 to 5% by mass based on the dimethylformamide.
Furthermore, the catalyst is dibutyltin dilaurate, and the adding amount of the catalyst is 0.5-6% of the mass of the N-carboxylic acylated chitosan.
Furthermore, the addition amount of the 4- (2, 3-epoxypropoxy) indole is 300-500% of the mass of the N-carboxylic acylated chitosan.
The invention firstly utilizes dibenzoyl tartaric acid to react with amino in the chitosan to prepare N-carboxylic acylated chitosan, introduces the dibenzoyl tartaric acid into the branched chain of the chitosan, destroys the compact structure of the chitosan, weakens the intermolecular hydrogen bonding effect, and improves the solubility of the chitosan in water and organic solvent; then, 4- (2, 3-epoxypropoxy) indole is used for further modifying chitosan, the 4- (2, 3-epoxypropoxy) indole and hydroxyl in the chitosan are subjected to O-alkylation reaction to obtain an alkylated chitosan derivative, the hydrogen bond effect among chitosan molecules is further destroyed, the solubility of the chitosan is further improved, strong hydrophilic groups such as carboxyl are introduced into the modified chitosan, the water absorption is improved, and the absorption of the material to water can be further improved by functional groups in dibenzoyl tartaric acid and a chitosan skeleton structure; the chitosan derivative is used for blending modification of polylactic acid, the defect of poor hygroscopicity of a polylactic acid material can be overcome, the permeability and moisture conductivity of polylactic acid fibers are improved, the air permeability is improved, and the strength and the toughness of the polylactic acid material can be improved. In addition, the chitosan material has good biocompatibility, and the fiber prepared by blending the chitosan material with polylactic acid is soft and fluffy in hand feeling and enhanced in comfort.
A chitosan derivative is prepared by the method.
Application of chitosan derivative in preparing polylactic acid fiber.
A preparation method of polylactic acid fiber comprises the following steps:
step one, uniformly mixing polylactic acid, polyvinyl alcohol, a chitosan derivative and an antioxidant to obtain a mixed material;
step two, preparing and obtaining nascent fiber by using a melt spinning method;
and step three, carrying out hot drawing and heat setting on the nascent fiber to obtain the polylactic acid fiber.
Further, the weight average molecular weight of the polylactic acid is 8 to 20 ten thousand, preferably 10 to 16 ten thousand.
Furthermore, the polymerization degree of the polyvinyl alcohol is 800-1200, the alcoholysis degree is 98%, and the addition amount of the polyvinyl alcohol is 6-10% of the mass of the polylactic acid.
Further, the addition amount of the chitosan derivative is 3-5% of the mass of the polylactic acid.
Further, the antioxidant is any one of tris (2, 4-di-tert-butylphenyl) phosphite, 2, 6-di-tert-butyl-4-methylphenol, dilauryl thiodipropionate and 4,4' -methylene bis (2, 6-di-tert-butylphenol), and the addition amount of the antioxidant is 0.8-2% of the mass of the polylactic acid.
Further, the melt spinning temperature is 180 to 250 ℃, preferably 200 to 220 ℃.
Further, the temperature of the hot drawing is 70-130 ℃, preferably 90-100 ℃; the draft ratio is 1 to 5 times, preferably 3 to 5 times.
Further, the heat setting temperature is 80-150 ℃, preferably 90-110 ℃.
The polylactic acid material has good moisture permeability, water diffusivity and antibacterial activity, is an ideal material for manufacturing the sanitary material, but has poor hygroscopicity, toughness and heat resistance, and is difficult to be made into fibers only by using the polylactic acid, so that the prepared sanitary material cannot be quickly absorbed when encountering a large amount of liquid; according to the invention, polylactic acid is used as a base material, and the chitosan derivative, polyvinyl alcohol and the antioxidant are added to prepare the polylactic acid fiber, so that the performance of the polylactic acid material is maintained, the advantages of the chitosan derivative are combined, the defect of poor hygroscopicity of the polylactic acid material is overcome, the moisture permeability and the air permeability of the polylactic acid fiber are improved, the degradation performance is improved, and the strength and the toughness of the polylactic acid fiber are enhanced.
The polylactic acid fiber prepared by the method.
Preparation of polylactic acid fiber for adult incontinenceThe application of the nursing pad comprises that polylactic acid fiber is used as a non-woven fabric material which is prepared by mixing, opening, cotton feeding, carding, direct net forming and hot rolling reinforcement, and is cut into the required size to be used as the surface layer of the adult incontinence nursing pad; the weight of the non-woven fabric material is 10-30g/m 2 The thickness is 0.05-0.3mm, and the hot rolling temperature is 110-140 ℃.
Further, in order to further enhance the mechanical property of the polylactic acid fiber and further enhance the service life and comfort of the adult incontinence nursing pad, before the polylactic acid fiber is made into a non-woven fabric material, the post-finishing is carried out by using a mixed solution containing 5-p-anisyl furfural, and the method specifically comprises the following steps:
adding surfactant, citric acid, and 5-p-anisyl furfural into deionized water, mixing, performing ultrasonic treatment at 50-60 deg.C for 30-50min, adding polylactic acid fiber into the mixed solution, stirring at 50-60 deg.C and 200-500r/min for 1-5h, filtering, washing with water for several times, and drying.
The surfactant is lauramidopropyl betaine, and the addition amount of the surfactant is 2-4% of the mass of the deionized water.
The addition amount of the citric acid is 1-2.5% of the mass of the deionized water.
The addition amount of the 5-p-anisyl furfural is 0.05-0.2% of the mass of the deionized water.
According to the invention, the polylactic acid fiber is subjected to after-treatment by using the mixed solution containing 5-p-anisyl furfural, and the aldehyde group in the 5-p-anisyl furfural and the amino group in the chitosan derivative are subjected to Schiff base reaction, so that the bonding fastness between the fibers is increased, the tensile property of the material is improved, and the fiber falling is reduced and the comfort level is increased in the use process of the adult incontinence nursing pad.
According to the invention, the chitosan derivative and the polylactic acid are mixed to prepare the polylactic acid fiber, and the polylactic acid fiber is prepared into the non-woven fabric material to be used as the surface layer of the adult incontinence nursing pad, so that the invention has the following beneficial effects: after the chitosan is modified by dibenzoyl tartaric acid and 4- (2, 3-epoxypropoxy) indole, the solubility and the hygroscopicity are improved, the polylactic acid is modified by the chitosan derivative in a blending way, the defect of poor hygroscopicity of the polylactic acid material can be overcome, the permeability, the moisture permeability and the air permeability of the polylactic acid fiber are improved, the degradation performance is improved, and the strength and the toughness of the polylactic acid material can be enhanced; the obtained polylactic acid fiber has soft hand feeling, fluffiness and strong comfort, and when the polylactic acid fiber is used for preparing the surface layer of sanitary materials such as adult incontinence nursing pads, liquid is quickly absorbed by contacting the surface layer, so that accumulation, side leakage and the like are avoided, and the applicability is strong.
Therefore, the invention provides polylactic acid fiber, and the polylactic acid fiber is made into a non-woven fabric material used as the surface layer of the adult incontinence nursing pad, the obtained non-woven fabric material has the tensile strength higher than 3.7N/5cm, the elongation at break higher than 41%, the strength is high, the toughness is good, and the moisture permeability is higher than 9600g/m 2 And d, high moisture permeability, air permeability of not less than 6000mm/s, good air permeability, degradation rate of 98.8 percent, strong comfort and excellent comprehensive performance.
Drawings
FIG. 1 is an FTIR chart of a chitosan derivative obtained in example 1;
FIG. 2 is a graphical representation of the results of tensile property testing of nonwoven materials;
FIG. 3 is a graphical representation of the results of a moisture vapor transmission rate test of a nonwoven material;
FIG. 4 is a graphical representation of the results of an air permeability test of a nonwoven material;
FIG. 5 is a graph showing the results of a degradation rate test of a nonwoven material.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1:
the present example provides a polylactic acid fiber, which is prepared by the following method:
step one, uniformly mixing 100 parts by weight of polylactic acid (with the weight-average molecular weight of 15 ten thousand), 8 parts by weight of polyvinyl alcohol (with the polymerization degree of 1000 and the alcoholysis degree of 98%), 4.2 parts by weight of chitosan derivative and 1 part by weight of 2, 6-di-tert-butyl-4-methylphenol to obtain a mixed material;
step two, preparing the mixed material obtained in the step one into nascent fiber by using a melt spinning method, wherein the melting temperature is 210 ℃;
and step three, carrying out hot drawing and heat setting on the nascent fiber obtained in the step two to obtain the polylactic acid fiber, wherein the hot drawing temperature is 95 ℃, the drawing multiple is 3 times, and the heat setting temperature is 100 ℃.
The chitosan derivative is prepared by the following method:
s1, adding 3 parts by weight of chitosan (the deacetylation degree is 90 percent, and the weight-average molecular weight is 6 ten thousand) into 100 parts by weight of dimethylformamide, adding 5.4 parts by weight of dibenzoyltartaric acid and 3.6 parts by weight of 1-ethyl-3 (3-dimethylaminopropyl) carbodiimide hydrochloride, and introducing N 2 Protecting, stirring at 120 deg.C and 1000r/min for reaction for 12 hr, adding excessive acetone for precipitation, washing with alcohol and ether for 5 times, and drying at 40 deg.C to obtain N-carboxyacylated chitosan;
s2, adding 3 parts by weight of N-carboxylic acylated chitosan into 100 parts by weight of dimethylformamide, adding 0.1 part by weight of dibutyltin dilaurate, stirring at 45 ℃ and 800r/min for reaction for 30min, then heating to 55 ℃, adding 12.6 parts by weight of 4- (2, 3-epoxy propoxy) indole, continuing stirring for 6h, after the reaction is finished, performing rotary evaporation, removing organic micromolecules and water, washing with acetone for 3 times, and drying at 40 ℃ to obtain the chitosan derivative.
The chitosan derivative obtained is tested by an infrared spectrometer, and an FTIR chart is shown in figure 1: as can be seen from the figure, in the chitosan spectrum, at 3400cm -1 An absorption peak of-OH in the vicinity of 1648cm -1 、1556cm -1 、1315cm -1 The characteristic absorption peak of amino near the amino is 1150cm -1 The nearby part is the stretching vibration peak of an ether oxygen bond, 1070cm -1 The nearby part is C-O stretching vibration, and the absorption peak is the characteristic peak of chitosan; in the spectrum of the chitosan derivative, 3400cm -1 The nearby strong absorption peak is due to the introduction of-OH after the epoxy reaction, 1450cm -1 、1240cm -1 Two strong absorption peaks appear nearby, which are caused by bending vibrations of C = O and-OH in the carboxyl group, 760cm -1 The results show that 4- (2, 3-epoxypropoxy) indole and dibenzoyl tartaric acid are successfully grafted on chitosan.
Example 2:
this example provides another polylactic acid fiber prepared in substantially the same manner as in example 1, except that the chitosan derivative was prepared in such amounts that the amounts of N-carboxyacylated chitosan and 4- (2, 3-epoxypropoxy) indole were 3 parts by weight and 7.5 parts by weight, respectively.
Example 3:
this example provides another polylactic acid fiber prepared in substantially the same manner as in example 1, except that the chitosan derivative was prepared in such amounts that the amounts of N-carboxyacylated chitosan and 4- (2, 3-epoxypropoxy) indole were 3 parts by weight and 9 parts by weight, respectively.
Example 4:
this example provides another polylactic acid fiber prepared in substantially the same manner as in example 1, except that the chitosan derivative was prepared in such amounts that the amounts of N-carboxyacylated chitosan and 4- (2, 3-epoxypropoxy) indole were 3 parts by weight and 15 parts by weight, respectively.
Example 5:
this example provides another polylactic acid fiber prepared in substantially the same manner as in example 1, except that the chitosan derivative was prepared in such amounts that the amounts of N-carboxyacylated chitosan and 4- (2, 3-epoxypropoxy) indole were 3 parts by weight and 16.5 parts by weight, respectively.
Example 6:
this example provides another polylactic acid fiber prepared substantially in the same manner as in example 1, except that the chitosan derivative is prepared by the following method:
adding 3 parts by weight of chitosan (degree of deacetylation is 90%, weight average molecular weight is 6 ten thousand) to 100 parts by weight of dimethylformamide, and adding 5.4 parts by weight of dibenzoyltartaric acid, 3.6 parts by weight of 1-ethyl-3 (3-dimethylaminopropyl) carbodiimide hydrochloride, N 2 Stirring at 120 deg.C and 1000r/min under protection for 12 hr, adding excessive acetone for precipitation, washing with alcohol and ether for 5 times, and drying at 40 deg.C.
Example 7:
this example provides another polylactic acid fiber, which is prepared substantially in the same manner as in example 1, except that the chitosan derivative is prepared by the following method:
adding 3 parts by weight of chitosan (the deacetylation degree is 90 percent, the weight average molecular weight is 6 ten thousand) into 100 parts by weight of dimethylformamide, adding 0.25 part by weight of dibutyltin dilaurate, stirring at 45 ℃ and 800r/min for reaction for 30min, then heating to 55 ℃, adding 12.6 parts by weight of 4- (2, 3-epoxy propoxy) indole, continuing stirring for 6h, after the reaction is finished, performing rotary evaporation to remove organic micromolecules and water, washing with acetone for 3 times, and drying at 40 ℃ to obtain the chitosan/N-acetyl-D-indole compound.
Example 8:
this example provides another polylactic acid fiber prepared in substantially the same manner as in example 1 except that the chitosan derivative was replaced with unmodified chitosan, the degree of deacetylation of chitosan was 90%, and the weight average molecular weight was 6 ten thousand.
Example 9:
this example provides another polylactic acid fiber prepared in substantially the same manner as in example 1, except that the chitosan derivative was not added in the first step.
Example 10:
this example provides another polylactic acid fiber, which is prepared in substantially the same manner as in example 1, except that the method further comprises the following steps:
mixing 3 parts by weight of lauramidopropyl betaine, 1.5 parts by weight of citric acid, 0.12 part by weight of 5-p-anisyl furfural and 100 parts by weight of deionized water, and performing ultrasonic treatment at 55 ℃ for 40min to obtain a mixed solution, wherein the ultrasonic frequency is 20kW, and the power density is 0.4W/cm 2 The polylactic acid fiber obtained in the example 1 is placed in the mixed solution, stirred for 3.5 hours at the temperature of 60 ℃ and at the speed of 500r/min, washed for 5 times by water and dried at the temperature of 40 ℃ to obtain the polylactic acid fiber.
Example 11:
this example provides another polylactic acid fiber prepared substantially in the same manner as in example 10, except that the mixed solution does not contain 5-p-anisyl furfural.
In order to verify the technical effect of the invention, the polylactic acid fibers obtained in the examples 1-11 are mixed, opened, fed with cotton, carded, directly laid, and subjected to hot rolling reinforcement at 120 ℃ to prepare a non-woven fabric material as a sample, wherein the gram weight of the non-woven fabric material is 20g/m 2 The thickness was 0.2mm, and the following tests were carried out.
Test example 1:
tensile property:
the nonwoven material was tested for tensile properties using an Instron3365 Universal materials tester (Instron, USA) at a tensile speed of 100mm/min with a holding gauge of 200mm and a pretension of 2N for 5 tests per sample, and the average was taken.
FIG. 2 is the results of the tensile properties test of the nonwoven materials, and it can be seen that the nonwoven materials obtained in preferred examples 1, 3 and 4 have a breaking strength of more than 3.7cN/dtex, an elongation at break of more than 41% and excellent tensile properties; comparing examples 1-9, examples 2 and 5, which show that the tensile properties of the nonwoven materials obtained from examples 1 are lower than those of example 1, and that the tensile properties of the nonwoven materials obtained from examples 6 and 7 are significantly different from those of example 1 and lower than those of examples 2 and 5, which show that the chitosan modified with dibenzoyl tartaric acid and 4- (2, 3-epoxypropoxy) indole is more helpful to improve the tensile properties of the nonwoven materials than the chitosan not completely modified, and that the tensile properties of the nonwoven materials obtained from examples 8 and 9 are lower than those of examples 6 and 7, and the tensile properties of the nonwoven materials obtained from example 8 are slightly higher than those of example 9, but smaller difference indicates that whether the addition of the chitosan not completely modified has a smaller influence on the tensile properties of the nonwoven materials; comparing examples 10 and 11, the tensile properties of the nonwoven material obtained in example 10 are higher than those of example 1, while the difference between the tensile properties of the nonwoven material obtained in example 11 and example 1 is smaller, which indicates that the polylactic acid fibers are helpful for further enhancing the tensile properties of the nonwoven material after being treated with the mixed solution containing 5-p-anisyl furfural.
Test example 2:
moisture permeability test:
the inverted cup method described in reference to the standard GB/T12704 adopts a moisture permeation test box to test the moisture permeation rate, the test time is 24h, each sample is tested for 5 times, and the average value is taken.
FIG. 3 shows the moisture permeability test results of the nonwoven fabric material, and it can be seen that the moisture permeability of the nonwoven fabric material obtained by the present invention is up to 9872.5g/m 2 And d, the moisture permeability is high, the moisture permeability of the nonwoven materials obtained in comparative examples 1-9 and examples 2 and 5 is lower than that of example 1, the moisture permeability is poorer than that of example 1, the moisture permeability of the nonwoven materials obtained in examples 6 and 7 has larger difference with that of example 1, the modification treatment of chitosan has larger influence on the moisture permeability of the nonwoven materials, the moisture permeability of the nonwoven materials obtained in examples 8 and 9 is obviously lower than that of example 1, and the moisture permeability of the nonwoven materials obtained in examples 8 and 9 is equivalent, and whether unmodified chitosan is added or not has almost no influence on the moisture permeability of the nonwoven materials.
Test example 3:
and (3) testing the air permeability:
the permeability test was carried out by using a YG461 type fabric permeability tester, with reference to the method for measuring the fabric-to-fabric permeability, with a test pressure of 60Pa, a nozzle diameter of 5mm, and each sample was tested 5 times, and the average value was taken.
FIG. 4 shows the results of air permeability test of nonwoven fabric material, and it can be seen that the nonwoven fabric material obtained in example 1 has an air permeability as high as 6180.5mm/s and is excellent in air permeability, and in comparative examples 1-5, it can be seen that the air permeability of the nonwoven fabric material obtained in the preparation process of chitosan derivative increases with the increase of the addition amount of 4- (2, 3-epoxypropoxy) indole; comparing examples 6 and 7, it can be seen that the chitosan modified by the two compounds is more beneficial to improving the air permeability of the non-woven fabric material compared with the chitosan modified by only using dibenzoyl tartaric acid or 4- (2, 3-epoxypropoxy) indole; comparing examples 8 and 9, it can be seen that the air permeability of the nonwoven fabric material obtained by adding the unmodified chitosan is equivalent to that of the nonwoven fabric material obtained by adding the unmodified chitosan, and both are lower than that of example 1, which indicates that the air permeability of the nonwoven fabric material is not obviously influenced by adding the chitosan.
Test example 4:
degradation performance:
the degradation rate of the non-woven fabric material is tested by reference to the standard GB/T19277.1-2011, each sample is tested for 5 times, and the average value is taken.
Fig. 5 is a result of a degradation rate test of a nonwoven fabric material, and it can be seen that the degradation rate of the nonwoven fabric materials obtained in preferred embodiments 1, 3 and 4 is as high as 97% or more, and the degradation performance is excellent, while the degradation rate of the nonwoven fabric materials obtained in embodiments 2 and 5 to 7 is significantly lower than that of embodiment 1, which indicates that the degradation performance of the nonwoven fabric material can be greatly improved after chitosan is modified by dibenzoyl tartaric acid and 4- (2, 3-epoxypropoxy) indole, and the degradation rate of the nonwoven fabric materials obtained in embodiments 8 and 9 is slightly different from that of the nonwoven fabric material obtained in embodiment 1, and significantly lower than that of the nonwoven fabric material obtained in embodiment 1, which indicates that chitosan is added to polylactic acid fiber without being modified, and has no significant influence on the degradation performance of the nonwoven fabric material.
While the invention has been described in detail in the foregoing by way of general description, and specific embodiments and experiments, it will be apparent to those skilled in the art that modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. This invention is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It will be understood that the invention is not limited to the precise arrangements that have been described above and shown in the drawings, and that various modifications and changes can be made without departing from the scope thereof.
Claims (7)
1. A method for preparing a chitosan derivative, which is characterized by comprising the following steps:
s1, adding chitosan into dimethyl formamideAdding dibenzoyl tartaric acid and water reducing agent after stirring uniformly, wherein the addition amount of dibenzoyl tartaric acid is 120-200% of the mass of chitosan, and introducing N 2 Protecting, stirring and reacting for 3-24h at 100-150 ℃ and 600-1500r/min, adding acetone for precipitation, washing with alcohol and ether for several times, and drying to obtain N-carboxyl acylation chitosan;
s2, adding N-carboxylic acylated chitosan into dimethylformamide, adding a catalyst, stirring and reacting for 20-50min at 40-50 ℃ and 600-1000r/min, then heating to 50-60 ℃, adding 4- (2, 3-epoxy propoxy) indole, wherein the addition amount of the 4- (2, 3-epoxy propoxy) indole is 300-500% of the mass of the N-carboxylic acylated chitosan, continuously stirring for 4-8h, after the reaction is finished, performing rotary evaporation to remove organic micromolecules and water, washing with acetone for several times, and drying to obtain the chitosan derivative.
2. The method as claimed in claim 1, wherein the chitosan has a weight average molecular weight of 3 to 10 ten thousand and a degree of deacetylation of 85% or more.
3. A chitosan derivative produced by the method according to any one of claims 1 to 2.
4. Use of the chitosan derivative of claim 3 in the preparation of polylactic acid fibers.
5. A preparation method of polylactic acid fiber is characterized by comprising the following steps:
step one, uniformly mixing polylactic acid, polyvinyl alcohol, the chitosan derivative of claim 3 and an antioxidant, wherein the addition amount of the chitosan derivative is 3-5% of the mass of the polylactic acid, so as to obtain a mixed material;
step two, preparing and obtaining nascent fiber by using a melt spinning method;
and step three, carrying out hot drawing and heat setting on the nascent fiber to obtain the polylactic acid fiber.
6. A polylactic acid fiber produced by the method according to claim 5.
7. The use of the polylactic acid fiber of claim 6 in the preparation of adult incontinence nursing pad, which comprises mixing, opening, cotton feeding, carding, direct web forming, hot rolling and reinforcing the polylactic acid fiber to obtain non-woven fabric material, cutting into required size as the surface layer of adult incontinence nursing pad; the weight of the non-woven fabric material is 10-30g/m 2 The thickness is 0.05-0.3mm, and the hot rolling temperature is 110-140 ℃.
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| JP2756060B2 (en) * | 1992-08-17 | 1998-05-25 | 大日精化工業株式会社 | Method for producing chitosan derivative |
| JP3731007B2 (en) * | 1994-12-12 | 2006-01-05 | 片倉チッカリン株式会社 | N-carboxyacyl chitosan and method for producing the same |
| JPH1036214A (en) * | 1996-07-24 | 1998-02-10 | Katakura Chitsukarin Kk | Base material for cosmetic |
| CN1325520C (en) * | 2003-12-22 | 2007-07-11 | 盐城工学院 | Preparation of double type amphoteric chitosan derivative |
| JP4866173B2 (en) * | 2006-01-25 | 2012-02-01 | 大日精化工業株式会社 | Hydroxyalkylated chitosan solution |
| CN101824160A (en) * | 2010-03-30 | 2010-09-08 | 东华大学 | Preparation method of chitosan/polyvinyl alcohol/polylactic acid blended porous membrane |
| CN101798403B (en) * | 2010-03-30 | 2012-02-01 | 东华大学 | Method for preparing chitosan/polyving alcohol/polylactic acid blended dense membrane |
| US9814786B2 (en) * | 2013-12-02 | 2017-11-14 | Nicolai Bovin | Functionalizing nanofibres |
| US11229721B2 (en) * | 2014-02-28 | 2022-01-25 | The University Of Memphis Research Foundation | Chitosan nanofiber compositions, compositions comprising modified chitosan, and methods of use |
| CN108559009A (en) * | 2017-09-26 | 2018-09-21 | 西南石油大学 | A kind of preparation method of phthaloyl chitosan |
| CN111662457B (en) * | 2020-06-09 | 2022-07-12 | 四川大学 | Polylactic acid grafted quaternized chitosan material, stereocomplex crystal nanofiber membrane thereof, and preparation methods and applications of polylactic acid grafted quaternized chitosan material and stereocomplex crystal nanofiber membrane |
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