Chitosan modified nylon fiber as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of fiber modification, and provides a chitosan modified nylon fiber as well as a preparation method and application thereof. The preparation method comprises the following steps: mixing chitosan with an acid solvent to obtain a chitosan solution; the preparation method comprises the following steps: soaking nylon fibers in a chitosan solution, and sequentially carrying out drying treatment and curing treatment after soaking is finished, so as to obtain the chitosan modified nylon fibers. Wherein the chitosan is a natural polysaccharide, is non-toxic and harmless and meets the environmental protection requirement, and meanwhile, harmful chemical substances are not used in the preparation process, so that the safety of the product is ensured; the chitosan modified nylon fiber has a remarkable antibacterial effect, and the chitosan coating on the surface of the nylon fiber can effectively inhibit growth and reproduction of various bacteria and fungi. The chitosan modified nylon fiber prepared by the invention can be widely applied to the fields of medical supply packaging or food packaging and the like, and has great market potential.

Description

Technical Field

[0001] The invention relates to the technical field of fiber modification, and in particular to a chitosan modified nylon fiber and a preparation method and application thereof. Background Art

[0002] Existing bio-based nylon materials have the advantages of being environmentally friendly and renewable, but their antibacterial properties are insufficient, which limits their application in the fields of medical treatment and food packaging. Chitosan has excellent biocompatibility, blood compatibility, safety and microbial degradability, and is widely used in the fields of medicine, food, chemical industry, cosmetics, water treatment, metal extraction and recovery. Loading chitosan onto bio-based nylon materials is expected to improve the performance of bio-based nylon materials. Therefore, it is of great significance to find a green, low-cost preparation process for modified nylon fibers with high chitosan loading. Summary of the invention

[0003] The purpose of the present invention is to overcome the problems existing in the prior art and provide a chitosan-modified nylon fiber and a preparation method and application thereof. Chitosan is applied to the antibacterial treatment of nylon fiber, which can retain the original excellent properties of nylon fiber on the one hand and give it good antibacterial function on the other hand.

[0004] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0005] The present invention provides a method for preparing chitosan modified nylon fiber, comprising the following steps:

[0006] (1) mixing chitosan with an acid solvent to obtain a chitosan solution;

[0007] (2) soaking the nylon fiber in a chitosan solution, and then performing a drying treatment and a curing treatment in sequence after the soaking is completed to obtain the chitosan-modified nylon fiber.

[0008] Preferably, the acid solvent in step (1) comprises an inorganic acid or an organic acid; the mass fraction of the acid solvent is 1 to 10%;

[0009] The inorganic acid includes hydrochloric acid solution or sulfuric acid solution; the organic acid includes formic acid solution, acetic acid solution, lactic acid solution, tartaric acid solution, malic acid solution, citric acid solution or gluconic acid solution.

[0010] Preferably, the mass fraction of the chitosan solution in step (1) is 0.5-3%.

[0011] Preferably, in step (2), the nylon fiber is pretreated before soaking, and the pretreatment comprises the following steps:

[0012] The nylon fiber is spun to obtain nylon cloth; the nylon cloth is sequentially washed with a sodium dodecyl sulfate solution, washed with ethanol, washed with water and dried to complete the pretreatment of the nylon fiber.

[0013] Preferably, the mass fraction of sodium dodecyl sulfate solution is 0.1-0.3%; the washing time of sodium dodecyl sulfate solution is 5-10 minutes; the washing time of ethanol is 5-10 minutes; the number of water washings is 2-3 times, and the time of each water washing is independently 8-12 minutes;

[0014] The drying temperature is 50-70° C., and the drying time is 10-30 minutes.

[0015] Preferably, the mass volume ratio of the nylon fiber and the chitosan solution in step (2) is 0.4-0.5 g: 70-90 mL;

[0016] The soaking temperature in step (2) is 20-30° C., and the soaking time is 3-5 hours.

[0017] Preferably, the wind speed of the drying treatment in step (2) is 0.8 to 1.2 m / s, the temperature of the drying treatment is 20 to 30° C., and the time of the drying treatment is 18 to 36 h.

[0018] Preferably, the curing temperature in step (2) is 30 to 50° C., and the curing time is 3 to 6 hours.

[0019] The invention also provides chitosan modified nylon fibers prepared by the preparation method of the chitosan modified nylon fibers.

[0020] The invention also provides application of the chitosan modified nylon fiber in medical product packaging or food packaging.

[0021] The beneficial effects of the present invention are:

[0022] The present invention provides a method for preparing chitosan-modified nylon fiber, comprising the following steps: mixing chitosan with an acid solvent to obtain a chitosan solution; soaking the nylon fiber in the chitosan solution, and performing a drying treatment and a curing treatment in sequence after the soaking to obtain the chitosan-modified nylon fiber. Among them, chitosan, as a natural polysaccharide, is non-toxic and harmless, meets environmental protection requirements, and no harmful chemicals are used in the preparation process, thereby ensuring the safety of the product; secondly, the polycationic properties of chitosan can react with acidic substances (such as teichoic acid, capsular polysaccharides, etc.) produced on the surface of bacteria, and adhere to the surface of bacteria, and react with bacterial cell membranes, thereby changing its permeability and causing a large amount of amino acids, proteins and other substances to leak, accelerating bacterial death. The chitosan-modified nylon fiber prepared by the present invention has a significant antibacterial effect, and the chitosan coating on the surface of the nylon fiber can effectively inhibit the growth and reproduction of a variety of bacteria and fungi. The obtained chitosan-modified nylon fiber can be widely used in the fields of medical supplies packaging or food packaging, and has great market potential. DETAILED DESCRIPTION

[0023] The present invention provides a method for preparing chitosan modified nylon fiber, comprising the following steps:

[0024] (1) mixing chitosan with an acid solvent to obtain a chitosan solution;

[0025] (2) soaking the nylon fiber in a chitosan solution, and then performing a drying treatment and a curing treatment in sequence after the soaking is completed to obtain the chitosan-modified nylon fiber.

[0026] In the present invention, the acid solvent in step (1) preferably comprises an inorganic acid or an organic acid; the mass fraction of the acid solvent is preferably 1 to 10%, more preferably 2 to 9%, and even more preferably 3 to 8%.

[0027] In the present invention, the inorganic acid preferably includes hydrochloric acid solution or sulfuric acid solution; the organic acid preferably includes formic acid solution, acetic acid solution, lactic acid solution, tartaric acid solution, malic acid solution, citric acid solution or gluconic acid solution.

[0028] In the present invention, the mixing in step (1) preferably comprises stirring and ultrasound performed sequentially, and the stirring temperature is preferably 20-30°C, more preferably 22-28°C, and more preferably 25-26°C; ultrasound is performed after uniform stirring, and the ultrasound temperature is preferably 20-30°C, more preferably 22-28°C, and more preferably 25-26°C; the ultrasound time is preferably 1-3h, more preferably 1.5-2.5h, and more preferably 2h.

[0029] In the present invention, the mass fraction of the chitosan solution in step (1) is preferably 0.5-3%, more preferably 1-2.5%, and more preferably 1.5-2%.

[0030] In the present invention, in step (2), the nylon fiber is preferably pretreated before soaking, and the purpose of the pretreatment is to improve the bonding force between chitosan and nylon fiber; the pretreatment preferably comprises the following steps:

[0031] The nylon fiber is spun to obtain nylon cloth; the nylon cloth is sequentially washed with a sodium dodecyl sulfate solution, washed with ethanol, washed with water and dried to complete the pretreatment of the nylon fiber.

[0032] In the present invention, weaving is accomplished by conventional techniques in the art, and the size (length×width) of the nylon cloth is preferably 3-7 cm×3-7 cm, more preferably 4-6 cm×4-6 cm, and more preferably 5 cm×5 cm.

[0033] In the present invention, during cleaning, there is no specific limitation on the amount of sodium dodecyl sulfate solution, ethanol and water, as long as the nylon cloth is completely immersed; the mass fraction of sodium dodecyl sulfate solution is preferably 0.1-0.3%, more preferably 0.15-0.25%, and more preferably 0.2%; the cleaning method of sodium dodecyl sulfate solution is preferably ultrasonic cleaning, and the cleaning time of sodium dodecyl sulfate solution is preferably 5-10 min, more preferably 6-9 min, and more preferably 7-8 min; the cleaning method of ethanol is preferably ultrasonic cleaning, and the cleaning time of ethanol is preferably 5-10 min, more preferably 6-9 min, and more preferably 7-8 min; the water washing method is preferably stirring cleaning, the number of water washings is preferably 2-3 times, and the time of each water washing is independently preferably 8-12 min, more preferably 9-11 min, and more preferably 10 min.

[0034] In the present invention, the drying temperature is preferably 50-70°C, more preferably 55-65°C, and more preferably 60°C; the drying time is preferably 10-30 min, more preferably 15-25 min, and more preferably 20 min.

[0035] In the present invention, the mass volume ratio of the nylon fiber and the chitosan solution in step (2) is preferably 0.4-0.5 g: 70-90 mL, more preferably 0.43-0.47 g: 75-85 mL, more preferably 0.44-0.45 g: 80-82 mL; the immersion temperature in step (2) is preferably 20-30°C, more preferably 22-28°C, more preferably 25-26°C; the immersion time is preferably 3-5 h, more preferably 3.5-4.5 h, more preferably 4 h.

[0036] In the present invention, the drying treatment in step (2) is preferably carried out in a fume hood, and the wind speed of the drying treatment is preferably 0.8 to 1.2 m / s, more preferably 0.9 to 1.1 m / s, and more preferably 1 m / s; the temperature of the drying treatment is preferably 20 to 30°C, more preferably 22 to 28°C, and more preferably 25 to 26°C; the time of the drying treatment is preferably 18 to 36 h, more preferably 22 to 32 h, and more preferably 24 to 26 h.

[0037] In the present invention, the curing temperature in step (2) is preferably 30-50°C, more preferably 35-45°C, and more preferably 40°C; the curing time is preferably 3-6h, more preferably 4-5h, and more preferably 4.5h.

[0038] The invention also provides chitosan modified nylon fibers prepared by the preparation method of the chitosan modified nylon fibers.

[0039] The invention also provides application of the chitosan modified nylon fiber in medical product packaging or food packaging.

[0040] The technical solutions provided by the present invention are described in detail below in conjunction with the embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0041] Example 1

[0042] Mixing chitosan and acetic acid solution, stirring at 25°C, and then ultrasonicating at 25°C for 2h to obtain a chitosan solution; wherein the mass fraction of the acetic acid solution is 2%, and the mass fraction of the chitosan solution is 0.5%;

[0043] The nylon fiber was spun to obtain a nylon cloth (5 cm×5 cm), the nylon cloth was immersed in a sodium dodecyl sulfate solution with a mass fraction of 0.2%, ultrasonically cleaned for 5 minutes, taken out and immersed in ethanol, ultrasonically cleaned for 5 minutes, and then immersed in water for washing, the washing method was stirring washing, the number of washing times was 3 times, the washing time of each time was independently 10 minutes, and finally dried at 60° C. for 20 minutes to obtain the pretreated nylon fiber;

[0044] 0.44 g of pretreated nylon fiber was immersed in 80 mL of chitosan solution at a temperature of 25°C for 3 h. After the immersion, it was placed in a fume hood and dried for 24 h at a wind speed of 1 m / s and a temperature of 25°C. Finally, it was cured in an oven at 37°C for 3 h to obtain chitosan-modified nylon fiber.

[0045] Example 2

[0046] The other conditions in Example 1 were kept unchanged, and the mass fraction of the chitosan solution was modified to 1% to obtain chitosan-modified nylon fibers.

[0047] Example 3

[0048] The other conditions in Example 1 were kept unchanged, and the mass fraction of the chitosan solution was modified to 2% to obtain chitosan-modified nylon fibers.

[0049] Example 4

[0050] The other conditions in Example 2 were kept unchanged, and the acetic acid solution was changed to a citric acid solution (the mass fraction of the citric acid solution was 2%) to obtain chitosan-modified nylon fibers.

[0051] Example 5

[0052] The other conditions in Example 2 were kept unchanged, and the acetic acid solution was changed to a hydrochloric acid solution (the mass fraction of the hydrochloric acid solution was 2%) to obtain chitosan-modified nylon fibers.

[0053] Comparative Example 1

[0054] The nylon fiber was spun to obtain a nylon cloth (5 cm×5 cm), which was immersed in a sodium dodecyl sulfate solution with a mass fraction of 0.2%, ultrasonically cleaned for 5 minutes, taken out and immersed in ethanol, ultrasonically cleaned for 5 minutes, and then immersed in water for washing. The washing method was stirring washing, the number of washing times was 3, and the washing time of each time was independently 10 minutes. Finally, the nylon cloth was dried at 60° C. for 20 minutes to obtain the pretreated nylon fiber.

[0055] The chitosan-modified nylon fibers prepared in Examples 1 to 5 and the pretreated nylon fibers prepared in Comparative Example 1 were respectively subjected to antibacterial zone diameter tests. The antibacterial zone diameter test method was as follows: 25 mL of agar medium was poured into sterile culture dishes in a clean bench and allowed to cool and solidify naturally; a pipette was used to take a 1×10 8 100 μL of Escherichia coli suspension with CFU / mL was inoculated on the culture medium and evenly smeared on the surface of the agar culture medium with a smear stick. The chitosan-modified nylon fibers prepared in Examples 1 to 5 and the pretreated nylon fibers prepared in Comparative Example 1 were cut into circular samples with a diameter of 20 mm, placed on the center surface of the agar culture medium, covered with a culture dish cover, inverted, and cultured in a 37°C incubator for 24 hours to observe the results. Through the above test, the performance test results of the chitosan-modified nylon fibers in Examples 1 to 5 and the pretreated nylon fibers in Comparative Example 1 were obtained, as shown in Table 1.

[0056] Table 1 Performance test results of chitosan modified nylon fibers in Examples 1 to 5 and pretreated nylon fibers in Comparative Example 1

[0057] Case Diameter of inhibition zone (mm) Example 1 3.0±0.2 Example 2 6.5±0.2 Example 3 6.1±0.3 Example 4 4.3±0.2 Example 5 5.8±0.2 Comparative Example 1 0

[0058] It can be seen from Table 1 that the antibacterial ability of chitosan modified nylon fiber is related to the mass fraction of chitosan solution and the type of acid solvent. By comparing Examples 1, 2, and 3, it can be seen that when the mass fraction of chitosan solution is 1%, the chitosan content loaded on the nylon fiber is the highest and the antibacterial effect is the best; by comparing Examples 2, 4, and 5, it can be seen that when acetic acid solution is selected as the acid solvent, the antibacterial effect is the most obvious.

[0059] As can be seen from the above embodiments, the present invention provides a method for preparing chitosan-modified nylon fiber, comprising the following steps: mixing chitosan with an acid solvent to obtain a chitosan solution; soaking the nylon fiber in the chitosan solution, and drying and curing the nylon fiber in sequence after the soaking to obtain the chitosan-modified nylon fiber. Among them, chitosan, as a natural polysaccharide, is non-toxic and harmless, meets environmental protection requirements, and no harmful chemicals are used in the preparation process, thereby ensuring the safety of the product; secondly, the polycationic properties of chitosan can react with acidic substances (such as teichoic acid, capsular polysaccharides, etc.) produced on the surface of bacteria, and adhere to the surface of bacteria, and react with bacterial cell membranes, thereby changing its permeability and causing a large amount of amino acids, proteins and other substances to leak, accelerating bacterial death. The chitosan-modified nylon fiber prepared by the present invention has a significant antibacterial effect, and the chitosan coating on the surface of the nylon fiber can effectively inhibit the growth and reproduction of a variety of bacteria and fungi. The obtained chitosan-modified nylon fiber can be widely used in the fields of medical supplies packaging or food packaging, and has great market potential.

[0060] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for preparing chitosan-modified nylon fiber, characterized in that: It includes the following steps: (1) mixing chitosan with an acid solvent to obtain a chitosan solution; (2) soaking the nylon fiber in a chitosan solution, and then performing a drying treatment and a curing treatment in sequence after the soaking is completed to obtain the chitosan-modified nylon fiber.

2. The method for preparing chitosan-modified nylon fiber according to claim 1, characterized in that: The acid solvent in step (1) comprises an inorganic acid or an organic acid; the mass fraction of the acid solvent is 1 to 10%; The inorganic acid includes hydrochloric acid solution or sulfuric acid solution; the organic acid includes formic acid solution, acetic acid solution, lactic acid solution, tartaric acid solution, malic acid solution, citric acid solution or gluconic acid solution.

3. The method for preparing chitosan-modified nylon fiber according to claim 2, characterized in that: The mass fraction of the chitosan solution in step (1) is 0.5-3%.

4. The method for preparing chitosan-modified nylon fiber according to claim 1, characterized in that: Step (2) The nylon fiber is pretreated before soaking, and the pretreatment comprises the following steps: The nylon fiber is spun to obtain nylon cloth; the nylon cloth is sequentially washed with a sodium dodecyl sulfate solution, washed with ethanol, washed with water and dried to complete the pretreatment of the nylon fiber.

5. The method for preparing chitosan-modified nylon fiber according to claim 4, characterized in that: The mass fraction of sodium dodecyl sulfate solution is 0.1-0.3%; the washing time of sodium dodecyl sulfate solution is 5-10 minutes; the washing time of ethanol is 5-10 minutes; the number of water washings is 2-3 times, and the time of each water washing is independently 8-12 minutes; The drying temperature is 50-70° C., and the drying time is 10-30 minutes.

6. The method for preparing chitosan-modified nylon fiber according to claim 1, characterized in that: The mass volume ratio of the nylon fiber and the chitosan solution in step (2) is 0.4-0.5 g: 70-90 mL; The soaking temperature in step (2) is 20-30° C., and the soaking time is 3-5 hours.

7. The method for preparing chitosan-modified nylon fiber according to claim 6, characterized in that: The wind speed of the drying process in step (2) is 0.8 to 1.2 m / s, the temperature of the drying process is 20 to 30° C., and the time of the drying process is 18 to 36 hours.

8. The method for preparing chitosan-modified nylon fiber according to claim 6 or 7, characterized in that: The curing temperature of step (2) is 30 to 50° C., and the curing time is 3 to 6 hours.

9. The chitosan-modified nylon fiber prepared by the method for preparing chitosan-modified nylon fiber according to any one of claims 1 to 8.

10. Use of the chitosan modified nylon fiber according to claim 9 in medical product packaging or food packaging.