An antibacterial polyester fiber and a method for preparing the same
By adding mugwort essential oil and initiator to ethyl acetate solution for grafting reaction, the antibacterial component is grafted onto polyester fiber, which solves the problem of short-lasting antibacterial effect of polyester fiber fabric and achieves long-term improvement of antibacterial performance.
Patent Information
- Application Number
- CN202411600821.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-11
- Publication Date
- 2025-10-24
- Estimated Expiration
- 2044-11-11
AI Technical Summary
In the prior art, the antibacterial effect of fabrics made of polyester fibers treated with finishing liquids is not long-lasting and decreases significantly with increasing number of washes.
Antibacterial ingredients such as terpineol and caryophyllene oxide were grafted onto polyester fibers by adding artemisia annua essential oil and initiators, including dicyclohexyl peroxydicarbonate, to ethyl acetate solution for a grafting reaction. Lauroyl peroxide and biphenyl were used in combination to improve the grafting efficiency and stability.
The durability of the antibacterial properties of polyester fiber fabrics was significantly improved, the antibacterial value did not change significantly before and after washing, and the antibacterial effect was significantly improved.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application belongs to the technical field of textiles, and particularly relates to an antibacterial polyester fiber and a preparation method thereof. BACKGROUND
[0002] Polyester fiber, commonly known as "polyester", is a synthetic fiber made of polyester raw material obtained by condensation of organic dihydric alcohol and aromatic dicarboxylic acid or ester thereof. Polyester fiber has the characteristics of appearance stiffness, good thermal stability (softening point is 230-240 DEG C, melting point is 255-265 DEG C, decomposition point is about 300 DEG C), high strength (dry state strength is 4-7 cN / dtex), high modulus (initial modulus can reach 14-17 GPa), moderate elongation (usually 20%-50%), excellent wrinkle resistance and shape retention, excellent elastic recovery performance, wear resistance, light resistance, non-matting and the like, and is commonly used in clothing, bedding, interior decoration and the like.
[0003] In recent years, with the improvement of living standards, people's functional requirements for textiles are no longer limited to comfort, and more and more consumers have higher requirements for the functionality of textiles, such as environmental protection and antibacterial properties.
[0004] In order to give the fabric made of polyester fiber antibacterial effect, people try to make the antibacterial agent into finishing liquor, and use the finishing liquor to finish the gray fabric made of polyester fiber. However, the antibacterial effect of the fabric made by this method is not durable, for example, the antibacterial effect decreases significantly with the increase of washing times. SUMMARY
[0005] Therefore, the purpose of the present application is to provide an antibacterial polyester fiber and a preparation method thereof, so as to solve the above-mentioned technical problems of poor durability of antibacterial effect of the fabric made by finishing the gray fabric made of polyester fiber with finishing liquor.
[0006] In order to achieve the above-mentioned purpose, the technical scheme of the present application is as follows:
[0007] In a first aspect, the present application provides a preparation method of an antibacterial polyester fiber, comprising the following steps:
[0008] S1. Adding essential oil of Artemisia argyi and initiator to ethyl acetate to obtain an ethyl acetate solution, wherein the initiator comprises dicyclohexyl peroxydicarbonate;
[0009] S2. Soaking the polyester fiber in m-cresol, then washing and drying, and then carrying out grafting reaction in the ethyl acetate solution under the atmosphere of protective gas, and then washing and drying to obtain the antibacterial polyester fiber.
[0010] Optionally, in step S1, the mass ratio of the essential oil of Artemisia argyi to the initiator is 1:0.003-0.006, preferably 1:0.004-0.006.
[0011] Optionally, in the ethyl acetate solution in step S1, the concentration of the essential oil of Artemisia argyi is 1wt%-3wt%, preferably 1.5wt%-3wt%.
[0012] Optionally, in step S1, the initiator further comprises lauryl peroxide.
[0013] Optionally, in step S1, the mass ratio of the lauryl peroxide to the dicyclohexyl peroxydicarbonate is 2-3:4-7, preferably 2.5-3:4-7.
[0014] Optionally, in the ethyl acetate solution in step S1, the solution further comprises biphenyl.
[0015] Optionally, in step S1, the mass ratio of the biphenyl to the essential oil of Artemisia argyi is 0.2-0.3:1, preferably 0.25-0.3:1.
[0016] Optionally, in step S2, the mass ratio of the m-cresol to the polyester fiber is 10-15:1.
[0017] Optionally, in step S2, the soaking time is 1.5-2.5h, preferably 2-2.5h.
[0018] Optionally, in step S2, the temperature of the grafting reaction is 60-80℃, preferably 65-80℃; the time of the grafting reaction is 1-3h, preferably 1.5-3h.
[0019] Optionally, in step S2, the mass ratio of the polyester fiber to the ethyl acetate solution is 1:15-20, preferably 1:16-20.
[0020] Optionally, in step S2, the temperature of the drying is 50-60℃, preferably 55-60℃; the time of the drying is 15-25min, preferably 20-25min.
[0021] In the second aspect, the present application further provides an antibacterial polyester fiber prepared by the method as described above.
[0022] As described above, the antibacterial polyester fiber and the preparation method thereof have the following beneficial effects:
[0023] In the present application, the initiator dicyclohexyl peroxydicarbonate is decomposed by heat to generate free radicals, which can initiate grafting reaction. Through grafting reaction, substances with antibacterial efficacy and containing alkenyl group in the essential oil of Artemisia argyi, such as terpineol and caryophyllene oxide, can be grafted onto the polyester fiber, i.e. substances with antibacterial efficacy in the essential oil of Artemisia argyi are introduced into the polyester fiber through chemical bonding, thereby improving the bonding strength between substances with antibacterial efficacy in the essential oil of Artemisia argyi and the polyester fiber, and further improving the antibacterial performance durability of the fabric made of the polyester fiber.
[0024] In the present application, lauryl peroxide is used in combination with dicyclohexyl peroxydicarbonate, which can improve the grafting efficiency, and further promote more substances such as terpineol and caryophyllene oxide to be grafted onto the polyester fiber, thereby improving the antibacterial effect of the fabric made of the polyester fiber.
[0025] In the present application, biphenyl can capture hydrogen radicals on the surface of the polyester, improve the stability of the hydrogen radicals, and be conducive to the formation of polyester radicals, so as to promote the reaction to proceed in the direction of grafting reaction, improve the grafting rate, and further improve the antibacterial effect of the fabric made of the polyester fiber. DETAILED DESCRIPTION
[0026] The present application is further described below through specific examples, but it should be pointed out that the specific material ratio, process conditions and results described in the embodiments of the present application are only used to illustrate the present application, and cannot limit the protection scope of the present application. Any equivalent changes or modifications made according to the spirit and principle of the present application should be covered within the protection scope of the present application. Unless otherwise specified, "wt%" in the present application refers to mass percentage.
[0027] An embodiment of the present application provides a preparation method of antibacterial polyester fiber, comprising the following steps:
[0028] S1. Essential oil of Artemisia argyi and an initiator are added to ethyl acetate to obtain an ethyl acetate solution with a concentration of 1wt%-3wt% of the essential oil of Artemisia argyi, and the mass ratio of the essential oil of Artemisia argyi to the initiator is 1:0.003-0.006, and the initiator comprises dicyclohexyl peroxydicarbonate;
[0029] S2. The polyester fiber is soaked in m-cresol with a mass of 10-15 times of the polyester fiber for 1.5-2.5h, then washed and dried, and then the polyester fiber is placed in ethyl acetate solution with a mass of 15-20 times of the polyester fiber in a protective gas atmosphere and subjected to grafting reaction at a temperature of 60-80℃ for 1-3h, then washed and dried at a temperature of 50-60℃ for 15-25min, to obtain the antibacterial polyester fiber.
[0030] In another exemplary embodiment of the present application, in step S1, the initiator further comprises lauryl peroxide, and the mass ratio of lauryl peroxide to dicyclohexyl peroxydicarbonate is 2-3:4-7.
[0031] In another exemplary embodiment of the present application, in the ethyl acetate solution of step S1, biphenyl is further included, and the mass ratio of biphenyl to essential oil of folium artemisiae argyi is 0.2-0.3:1.
[0032] Another embodiment of the present application further provides an antibacterial polyester fiber prepared according to the method as described above.
[0033] The present application will be described in detail below through specific exemplary embodiments. It should also be understood that the following embodiments are only used to specifically describe the present application, and cannot be understood as limiting the protection scope of the present application. Some non-essential improvements and adjustments made by those skilled in the art according to the above content of the present application all belong to the protection scope of the present application. The following exemplary specific process parameters are only one example in the appropriate range, i.e., those skilled in the art can make appropriate selection within the range through the description herein, and are not limited to the specific values of the following examples.
[0034] Example 1
[0035] A preparation method of an antibacterial polyester fiber, and the specific steps are as follows:
[0036] S1. Essential oil of folium artemisiae argyi (commercially available) and initiator dicyclohexyl peroxydicarbonate are added into ethyl acetate, and stirred uniformly to obtain an ethyl acetate solution with a concentration of 1wt% of essential oil of folium artemisiae argyi, and the mass ratio of essential oil of folium artemisiae argyi to initiator dicyclohexyl peroxydicarbonate is 1:0.006;
[0037] S2. The polyester fiber is soaked in m-cresol with a mass of 15 times of the polyester fiber for 2.5h, and then washed with clean water for 2 times, each for 4min, and dried, and then the polyester fiber is placed in the ethyl acetate solution (the mass ratio of polyester fiber to ethyl acetate solution is 1:15) under the atmosphere of nitrogen gas, and subjected to grafting reaction at a temperature of 80℃ for 1h, and then washed with clean water for 2 times, each for 6min, and then dried at a temperature of 50℃ for 25min to obtain the antibacterial polyester fiber.
[0038] Example 2
[0039] A preparation method of an antibacterial polyester fiber, and the specific steps are as follows:
[0040] S1. Essential oil of folium artemisiae argyi (commercially available) and initiator dicyclohexyl peroxydicarbonate are added into ethyl acetate, and stirred uniformly to obtain an ethyl acetate solution with a concentration of 3wt% of essential oil of folium artemisiae argyi, and the mass ratio of essential oil of folium artemisiae argyi to initiator dicyclohexyl peroxydicarbonate is 1:0.003;
[0041] S2. The polyester fiber was immersed in m-cresol at 10 times the mass of the polyester fiber for 1.5 hours, then washed with clean water 3 times for 5 minutes each time, dried, then the polyester fiber was placed in an ethyl acetate solution (mass ratio of polyester fiber to ethyl acetate solution was 1:20) under a nitrogen gas atmosphere at a temperature of 60°C for a grafting reaction for 3 hours, then washed with clean water 3 times for 5 minutes each time, then dried at a temperature of 60°C for 15 minutes to produce the antibacterial polyester fiber.
[0042] Example 3
[0043] A method for preparing an antibacterial polyester fiber, the specific steps being as follows:
[0044] S1. Ai Ye essential oil (commercially available) and an initiator, dicumyl peroxide and dicyclohexyl peroxydicarbonate, were added to ethyl acetate, stirred to obtain a 2wt% ethyl acetate solution of Ai Ye essential oil, the mass ratio of Ai Ye essential oil to initiator being 1:0.005.
[0045] S2. The polyester fiber was immersed in m-cresol at 12 times the mass of the polyester fiber for 2 hours, then washed with clean water 2 times for 5 minutes each time, dried, then the polyester fiber was placed in an ethyl acetate solution (mass ratio of polyester fiber to ethyl acetate solution was 1:18) under a nitrogen gas atmosphere at a temperature of 70°C for a grafting reaction for 2 hours, then washed with clean water 3 times for 5 minutes each time, then dried at a temperature of 54°C for 20 minutes to produce the antibacterial polyester fiber.
[0046] Example 4
[0047] The antibacterial polyester fiber was prepared in the same manner as Example 3, except for the following conditions:
[0048] S1. Ai Ye essential oil (commercially available) and an initiator, dicumyl peroxide and dicyclohexyl peroxydicarbonate, were added to ethyl acetate, stirred to obtain a 2wt% ethyl acetate solution of Ai Ye essential oil, the mass ratio of Ai Ye essential oil to initiator being 1:0.005.
[0049] Example 5
[0050] The antibacterial polyester fiber was prepared in the same manner as Example 3, except for the following conditions:
[0051] S1. Ai Ye essential oil (commercially available) and an initiator, dicumyl peroxide and dicyclohexyl peroxydicarbonate, were added to ethyl acetate, stirred to obtain a 2wt% ethyl acetate solution of Ai Ye essential oil, the mass ratio of Ai Ye essential oil to initiator being 1:0.005.
[0052] Example 6
[0053] Antibacterial polyester fibers were prepared in the same manner as Example 3 except for the following conditions:
[0054] S1. Add essential oil of Artemisia argyi (commercially available), initiator dicyclohexyl peroxydicarbonate and biphenyl to ethyl acetate, stir to obtain a solution of essential oil of Artemisia argyi in ethyl acetate with a concentration of 2 wt%, the mass ratio of essential oil of Artemisia argyi to initiator dicyclohexyl peroxydicarbonate being 1:0.005, and the mass ratio of biphenyl to essential oil of Artemisia argyi being 0.2:1.
[0055] Example 7
[0056] Antibacterial polyester fibers were prepared in the same manner as Example 3 except for the following conditions:
[0057] S1. Add essential oil of Artemisia argyi (commercially available), initiator dicyclohexyl peroxydicarbonate and biphenyl to ethyl acetate, stir to obtain a solution of essential oil of Artemisia argyi in ethyl acetate with a concentration of 2 wt%, the mass ratio of essential oil of Artemisia argyi to initiator dicyclohexyl peroxydicarbonate being 1:0.005, and the mass ratio of biphenyl to essential oil of Artemisia argyi being 0.3:1.
[0058] Comparative Example 1
[0059] Polyester fibers of the same origin as Example 1, which were not treated in any way.
[0060] Antibacterial performance test
[0061] The antibacterial polyester fibers prepared in Examples 1-7 and the polyester fibers of Comparative Example 1 were each made into a fabric, and 10 cm*10 cm samples were taken, and the antibacterial values of each sample against Staphylococcus aureus (ATCC 6538) and Escherichia coli (ATCC 1122938) were tested in accordance with GB / T 20944.2-2007 Textiles-Evaluation of antibacterial properties-Part 2: Absorption method, wherein the test bacterial solution was prepared after being cultured according to the culture C method, and the results are shown in Table 1.
[0062] Subsequently, each group of samples was machine washed at room temperature, the washing time was 10 min, the water level was full water level, the stirring speed was 180 r / min, the spin-drying speed was 650 r / min, the spin-drying time was 6 min, and then natural air drying was performed, and this cycle of washing-air drying was repeated 50 times. Then, the antibacterial values of each sample against Staphylococcus aureus (ATCC 6538) and Escherichia coli (ATCC 1122938) were tested again in accordance with GB / T 20944.2-2007 Textiles-Evaluation of antibacterial properties-Part 2: Absorption method, and the results are shown in Table 1.
[0063] Table 1: Results of antibacterial performance test
[0064]
[0065] As shown in Table 1, the antibacterial values of the fabric made of the antibacterial polyester fiber of Examples 1-7 to Staphylococcus aureus and Escherichia coli do not change significantly before and after washing. The results show that in the present application, the initiator dicyclohexyl peroxydicarbonate is decomposed to generate free radicals by heating, the free radicals can initiate grafting reaction, and through grafting reaction, substances such as terpineol and caryophyllene oxide with antibacterial efficacy and containing alkenyl in the leaf of Artemisia argyi can be grafted onto the polyester fiber, i.e. substances such as terpineol and caryophyllene oxide with antibacterial efficacy in the leaf of Artemisia argyi are introduced into the polyester fiber through chemical bonding, the bonding strength between substances such as terpineol and caryophyllene oxide with antibacterial efficacy in the leaf of Artemisia argyi and the polyester fiber is improved, and the antibacterial performance durability of the fabric made of the polyester fiber is improved.
[0066] As shown in Table 1, compared with Example 3, the antibacterial values of the fabric made of the antibacterial polyester fiber of Examples 4 and 5 to Staphylococcus aureus and Escherichia coli are significantly improved before washing. The results show that in the present application, the use of lauroyl peroxide and dicyclohexyl peroxydicarbonate in combination can improve the grafting efficiency, and thus more substances such as terpineol and caryophyllene oxide are grafted onto the polyester fiber, thereby improving the antibacterial effect of the fabric made of the polyester fiber.
[0067] As shown in Table 1, compared with Example 3, the antibacterial values of the fabric made of the antibacterial polyester fiber of Examples 6 and 7 to Staphylococcus aureus and Escherichia coli are significantly improved before washing. The results show that in the present application, biphenyl can capture hydrogen radicals on the surface of the polyester, improve the stability of the hydrogen radicals, be conducive to the formation of polyester radicals, promote the reaction to proceed in the direction of grafting reaction, improve the grafting rate, and thus improve the antibacterial effect of the fabric made of the polyester fiber.
[0068] The above examples only exemplarily illustrate the principles and effects of the present application, and are not used to limit the present application. Any person skilled in the art can modify or change the above examples without departing from the spirit and scope of the present application. Therefore, all equivalent modifications or changes completed by those skilled in the art without departing from the spirit and technical thought disclosed by the present application should be covered by the claims of the present application.
Claims
1. A method for producing an antibacterial polyester fiber, characterized by, The method comprises the following steps: S1. Adding essential oil of Artemisia argyi, initiator and biphenyl into ethyl acetate to obtain an ethyl acetate solution, wherein the initiator comprises dicyclohexyl peroxydicarbonate, and the mass ratio of the biphenyl to the essential oil of Artemisia argyi is 0.2-0.3:1; S2. Soaking the polyester fiber in m-cresol, then washing and drying, and then placing the polyester fiber in the ethyl acetate solution in a protective gas atmosphere to perform a grafting reaction, and then washing and drying to obtain the antibacterial polyester fiber.
2. The production method according to claim 1, characterized by, In step S1, the mass ratio of the essential oil of Artemisia argyi to the initiator is 1:0.003-0.006; And / or, in the ethyl acetate solution of step S1, the concentration of the essential oil of Artemisia argyi is 1wt%-3wt%.
3. The production method according to claim 1, characterized by, In step S1, the initiator further comprises lauryl peroxide.
4. The production method according to claim 3, characterized by, In step S1, the mass ratio of the lauryl peroxide to the dicyclohexyl peroxydicarbonate is 2-3:4-7.
5. The preparation method according to claim 1, characterized in that In step S2, the mass ratio of the m-cresol to the polyester fiber is 10-15:1; And / or, in step S2, the soaking time is 1.5-2.5h.
6. The method of claim 1, wherein, In step S2, the grafting reaction temperature is 60-80℃, and the grafting reaction time is 1-3h.
7. The preparation method according to claim 1, characterized in that In step S2, the mass ratio of the polyester fiber to the ethyl acetate solution is 1:15-20; And / or, in step S2, the drying temperature is 50-60℃, and the drying time is 15-25min.
8. The antibacterial polyester fiber prepared by the method according to any one of claims 1-7.
Citation Information
Patent Citations
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CN102863575A
An antibacterial textile product and a preparing method thereof
CN107044053A