Antibacterial polyester fiber and preparation method thereof

Abstract

The invention relates to an antibacterial polyester fiber and a preparation method thereof. The preparation method of the antibacterial polyester fiber comprises the following steps that S1, folium artemisiae argyi essential oil and an initiator are added into ethyl acetate, an ethyl acetate solution is obtained, and the initiator comprises dicyclohexyl peroxydicarbonate; s2, the polyester fibers are placed in m-cresol to be soaked and then washed and dried, then the polyester fibers are placed in an acetic ether solution under the protective gas atmosphere to be subjected to a grafting reaction, then washing and drying are conducted, and the antibacterial polyester fibers are prepared. According to the invention, terpilenol, caryophyllene oxide and other substances with an antibacterial effect in the folium artemisiae argyi essential oil are introduced into the polyester fiber in a chemical combination manner, so that the bonding strength between the terpilenol, caryophyllene oxide and other substances with the antibacterial effect and the polyester fiber is improved; furthermore, the durability of the antibacterial property of the fabric made of the polyester fiber is improved.

Description

Technical Field

[0001] The invention belongs to the technical field of textiles, and particularly relates to an antibacterial polyester fiber and a preparation method thereof. Background Art

[0002] Polyester fiber, commonly known as "polyester", is a synthetic fiber made of polyester raw materials formed by polycondensation of organic diols and aromatic dicarboxylic acids or their esters. Polyester fiber has a crisp appearance, good thermal stability (softening point is 230-240℃, melting point is 255-265℃, and decomposition point is about 300℃), high strength (strength in dry state is 4-7cN / dtex), high modulus (initial modulus can reach 14-17GPa), moderate elongation (usually 20%-50%), excellent wrinkle resistance and shape retention, excellent elastic recovery performance, wear resistance, light resistance, non-sticky hair, etc., and is often used in clothing, bedding, interior decoration and other fields.

[0003] In recent years, with the improvement of living standards, people's requirements for the functions of textiles are no longer limited to comfort. More and more consumers have put forward higher requirements for the functionality of textiles, such as environmental protection and antibacterial properties.

[0004] In order to give polyester fabrics antibacterial properties, people have tried to make antibacterial agents into finishing liquids and use the finishing liquids to post-finish polyester fabrics. However, the antibacterial properties of fabrics made in this way are not durable. For example, the antibacterial effect decreases significantly with the increase in the number of washings. Summary of the invention

[0005] In view of this, the object of the present invention is to provide an antibacterial polyester fiber and a preparation method thereof, so as to solve the technical problems such as the poor durability of the antibacterial effect of the fabric produced by post-finishing the grey cloth made of polyester fiber with a finishing liquid.

[0006] To achieve the above-mentioned object of the invention, the technical solution of the present invention is as follows:

[0007] In a first aspect, the present invention provides a method for preparing an antibacterial polyester fiber, comprising the following steps:

[0008] S1. Adding wormwood essential oil and an initiator to ethyl acetate to obtain an ethyl acetate solution, wherein the initiator comprises dicyclohexyl peroxydicarbonate;

[0009] S2. The polyester fiber is soaked in m-cresol, washed, and dried, and then placed in the ethyl acetate solution under a protective gas atmosphere for grafting reaction, and then washed and dried to obtain the antibacterial polyester fiber.

[0010] Optionally, in step S1, the mass ratio of the wormwood essential oil 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 wormwood essential oil is 1wt%-3wt%, preferably 1.5wt%-3wt%.

[0012] Optionally, in step S1, the initiator further includes lauroyl peroxide.

[0013] Optionally, in step S1, the mass ratio of lauroyl peroxide to dicyclohexyl peroxydicarbonate is 2-3:4-7, preferably 2.5-3:4-7.

[0014] Optionally, the ethyl acetate solution in step S1 also includes biphenyl.

[0015] Optionally, in step S1, the mass ratio of biphenyl to wormwood essential oil is 0.2-0.3:1, preferably 0.25-0.3:1.

[0016] Optionally, in step S2, the mass ratio of m-cresol to polyester fiber is 10-15:1.

[0017] Optionally, in step S2, the soaking time is 1.5-2.5 hours, preferably 2-2.5 hours.

[0018] Optionally, in step S2, the temperature of the grafting reaction is 60-80°C, preferably 65-80°C; the duration 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 drying temperature is 50-60°C, preferably 55-60°C; the drying time is 15-25 min, preferably 20-25 min.

[0021] Second, the present invention also provides an antibacterial polyester fiber prepared according to the method as described above.

[0022] As described above, the antibacterial polyester fiber and the preparation method thereof of the present invention have the following beneficial effects:

[0023] In the present invention, the initiator dicyclohexyl peroxydicarbonate decomposes under heat to generate free radicals, and the free radicals can initiate a grafting reaction. Through the grafting reaction, substances such as terpineol and caryophyllene oxide with antibacterial efficacy and containing alkenyl groups in the wormwood essential oil can be grafted onto the polyester fiber, that is, substances such as terpineol and caryophyllene oxide with antibacterial efficacy in the wormwood essential oil are introduced into the polyester fiber through chemical bonding, thereby improving the bonding strength between substances such as terpineol and caryophyllene oxide with antibacterial efficacy in the wormwood essential oil and the polyester fiber, thereby improving the durability of the antibacterial performance of the fabric made of the polyester fiber.

[0024] In the present invention, lauroyl peroxide and dicyclohexyl peroxydicarbonate are used in combination to improve the grafting efficiency, thereby promoting 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 invention, biphenyl can capture hydrogen radicals on the surface of polyester, improve the stability of hydrogen radicals, facilitate the formation of polyester radicals, promote the reaction in the direction of grafting reaction, increase the grafting rate, and further improve the antibacterial effect of the fabric made of polyester fiber. DETAILED DESCRIPTION

[0026] The present invention is further described below by specific examples, but it should be noted that the specific material ratios, process conditions and results described in the embodiments of the present invention are only used to illustrate the present invention and cannot be used to limit the protection scope of the present invention. All equivalent changes or modifications made according to the spirit of the present invention should be included in the protection scope of the present invention. Unless otherwise specified, in the present invention, "wt%" refers to mass percentage.

[0027] An embodiment of the present invention provides a method for preparing an antibacterial polyester fiber, comprising the following steps:

[0028] S1. Adding wormwood essential oil and an initiator to ethyl acetate to obtain an ethyl acetate solution having a concentration of 1wt%-3wt% of wormwood essential oil, the mass ratio of wormwood essential oil to the initiator being 1:0.003-0.006, the initiator comprising dicyclohexyl peroxydicarbonate;

[0029] S2. Soak the polyester fiber in 10-15 times its mass of m-cresol for 1.5-2.5 hours, wash and dry it, then place the polyester fiber in 15-20 times its mass of ethyl acetate solution under a protective gas atmosphere at 60-80°C for grafting reaction for 1-3 hours, then wash it, and dry it at 50-60°C for 15-25 minutes to obtain the antibacterial polyester fiber.

[0030] In another exemplary embodiment of the present invention, in step S1, the initiator further includes lauroyl peroxide, and the mass ratio of lauroyl peroxide to dicyclohexyl peroxydicarbonate is 2-3:4-7.

[0031] In another exemplary embodiment of the present invention, the ethyl acetate solution in step S1 further includes biphenyl, and the mass ratio of biphenyl to wormwood essential oil is 0.2-0.3:1.

[0032] Another embodiment of the present invention also provides an antibacterial polyester fiber prepared according to the method as described above.

[0033] The present invention is described in detail below by specific examples. It should also be understood that the following examples are only used to specifically illustrate the present invention and cannot be understood as limiting the scope of protection of the present invention. Some non-essential improvements and adjustments made by those skilled in the art based on the above content of the present invention belong to the scope of protection of the present invention. The specific process parameters and the like in the following examples are also only examples within a suitable range, that is, those skilled in the art can make a selection within a suitable range through the description herein, and are not limited to the specific values ​​​​exemplified below.

[0034] Example 1

[0035] A method for preparing an antibacterial polyester fiber, the specific steps are as follows:

[0036] S1. Add wormwood essential oil (commercially available) and dicyclohexyl peroxydicarbonate as an initiator to ethyl acetate, stir evenly, and obtain a 1wt% ethyl acetate solution of wormwood essential oil, the mass ratio of wormwood essential oil to initiator dicyclohexyl peroxydicarbonate is 1:0.006;

[0037] S2. Soak the polyester fiber in 15 times its mass of meta-cresol for 2.5 hours, then wash it with clean water twice, 4 minutes each time, and dry it. Then, place the polyester fiber in ethyl acetate solution (the mass ratio of polyester fiber to ethyl acetate solution is 1:15) under nitrogen gas atmosphere at 80°C for grafting reaction for 1 hour, then wash it with clean water twice, 6 minutes each time, and then dry it at 50°C for 25 minutes to obtain antibacterial polyester fiber.

[0038] Example 2

[0039] A method for preparing an antibacterial polyester fiber, the specific steps are as follows:

[0040] S1. Add wormwood essential oil (commercially available) and dicyclohexyl peroxydicarbonate as an initiator to ethyl acetate, stir evenly, and obtain a 3wt% ethyl acetate solution of wormwood essential oil, the mass ratio of wormwood essential oil to initiator dicyclohexyl peroxydicarbonate is 1:0.003;

[0041] S2. Soak the polyester fiber in 10 times its mass of meta-cresol for 1.5 hours, then wash it with clean water three times, each time for 5 minutes, and dry it. Then, place the polyester fiber in ethyl acetate solution (the mass ratio of polyester fiber to ethyl acetate solution is 1:20) under nitrogen gas atmosphere at 60°C for grafting reaction for 3 hours, then wash it with clean water three times, each time for 5 minutes, and then dry it at 60°C for 15 minutes to obtain antibacterial polyester fiber.

[0042] Example 3

[0043] A method for preparing an antibacterial polyester fiber, the specific steps are as follows:

[0044] S1. Add wormwood essential oil (commercially available) and dicyclohexyl peroxydicarbonate as an initiator to ethyl acetate, stir evenly, and obtain a 2wt% ethyl acetate solution of wormwood essential oil, the mass ratio of wormwood essential oil to initiator dicyclohexyl peroxydicarbonate is 1:0.005;

[0045] S2. Soak the polyester fiber in 12 times its mass of meta-cresol for 2 hours, then wash it with clean water twice, each time for 5 minutes, and dry it. Then, place the polyester fiber in ethyl acetate solution (the mass ratio of polyester fiber to ethyl acetate solution is 1:18) under nitrogen gas atmosphere at 70°C for grafting reaction for 2 hours, then wash it with clean water three times, each time for 5 minutes, and then dry it at 54°C for 20 minutes to obtain antibacterial polyester fiber.

[0046] Example 4

[0047] The antibacterial polyester fiber was prepared in the same manner as in Example 3 except for the following conditions:

[0048] S1. Add wormwood essential oil (commercially available) and an initiator to ethyl acetate, stir evenly, and obtain an ethyl acetate solution with a concentration of 2wt% of wormwood essential oil, the mass ratio of wormwood essential oil to initiator is 1:0.005, and the initiator is composed of lauroyl peroxide and dicyclohexyl peroxydicarbonate in a mass ratio of 2:7.

[0049] Example 5

[0050] The antibacterial polyester fiber was prepared in the same manner as in Example 3 except for the following conditions:

[0051] S1. Add wormwood essential oil (commercially available) and an initiator to ethyl acetate, stir evenly, and obtain an ethyl acetate solution with a concentration of 2wt% of wormwood essential oil, the mass ratio of wormwood essential oil to initiator is 1:0.005, and the initiator is composed of lauroyl peroxide and dicyclohexyl peroxydicarbonate in a mass ratio of 3:4.

[0052] Example 6

[0053] The antibacterial polyester fiber was prepared in the same manner as in Example 3 except for the following conditions:

[0054] S1. Add wormwood essential oil (commercially available), initiator dicyclohexyl peroxydicarbonate and biphenyl to ethyl acetate, stir evenly to obtain an ethyl acetate solution with a concentration of 2wt% of wormwood essential oil, the mass ratio of wormwood essential oil to initiator dicyclohexyl peroxydicarbonate is 1:0.005, and the mass ratio of biphenyl to wormwood essential oil is 0.2:1.

[0055] Example 7

[0056] The antibacterial polyester fiber was prepared in the same manner as in Example 3 except for the following conditions:

[0057] S1. Add wormwood essential oil (commercially available), initiator dicyclohexyl peroxydicarbonate and biphenyl to ethyl acetate, stir evenly to obtain an ethyl acetate solution with a concentration of 2wt% of wormwood essential oil, the mass ratio of wormwood essential oil to initiator dicyclohexyl peroxydicarbonate is 1:0.005, and the mass ratio of biphenyl to wormwood essential oil is 0.3:1.

[0058] Comparative Example 1

[0059] The polyester fiber is from the same source as that in Example 1 and is not subjected to any treatment.

[0060] Antibacterial performance testing

[0061] The antibacterial polyester fibers prepared in Examples 1-7 and the polyester fibers in Comparative Example 1 were made into fabrics, and 10 cm*10 cm samples were taken from each sample. The antibacterial value of each sample against Staphylococcus aureus (ATCC 6538) and Escherichia coli (ATCC 1122938) was tested according to "GB / T 20944.2-2007 Evaluation of Antibacterial Properties of Textiles 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 minutes, the water level was full, the stirring speed was 180r / min, the spin speed was 650r / min, the spin time was 6 minutes, and then naturally air-dried. After 50 cycles of washing and air-drying, 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 Evaluation of antibacterial properties of textiles Part 2: Absorption method", and the results are shown in Table 1.

[0063] Table 1 Antibacterial performance test results

[0064]

[0065] As shown in Table 1, before and after washing, the antibacterial values ​​of the fabrics made of the antibacterial polyester fibers of Examples 1-7 against Staphylococcus aureus and Escherichia coli did not change significantly. This result shows that in the present invention, the initiator dicyclohexyl peroxydicarbonate is decomposed by heat to generate free radicals, and the free radicals can initiate a grafting reaction. Through the grafting reaction, the antibacterial and alkenyl-containing substances such as terpineol and caryophyllene oxide in the wormwood essential oil can be grafted onto the polyester fiber, that is, the antibacterial substances such as terpineol and caryophyllene oxide in the wormwood essential oil are introduced into the polyester fiber through chemical bonding, thereby improving the bonding strength between the antibacterial substances such as terpineol and caryophyllene oxide in the wormwood essential oil and the polyester fiber, thereby improving the durability of the antibacterial performance of the fabrics made of polyester fibers.

[0066] As shown in Table 1, for the samples before washing, the antibacterial values ​​of the fabrics made of the antibacterial polyester fibers of Examples 4 and 5 against Staphylococcus aureus and Escherichia coli were significantly improved compared with Example 3. This result shows that in the present invention, the compound use of lauroyl peroxide and dicyclohexyl peroxydicarbonate can improve the grafting efficiency, thereby promoting more substances such as terpineol and caryophyllene oxide to be grafted onto the polyester fiber, thereby improving the antibacterial effect of the fabrics made of polyester fibers.

[0067] As shown in Table 1, for the samples before washing, the antibacterial values ​​of the fabrics made of the antibacterial polyester fibers of Examples 6 and 7 against Staphylococcus aureus and Escherichia coli were significantly improved compared with Example 3. This result shows that in the present invention, biphenyl can capture hydrogen free radicals on the surface of polyester, improve the stability of hydrogen free radicals, facilitate the formation of polyester free radicals, promote the reaction in the direction of grafting reaction, increase the grafting rate, and thus improve the antibacterial effect of the fabrics made of polyester fibers.

[0068] The above embodiments are merely illustrative of the principles and effects of the present invention, and are not intended to limit the present invention. Anyone familiar with the art may modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by a person of ordinary skill in the art without departing from the spirit and technical concept disclosed by the present invention shall still be covered by the claims of the present invention.

Claims

1. A method for preparing an antibacterial polyester fiber, characterized in that: The following steps are involved: S1. Adding wormwood essential oil and an initiator to ethyl acetate to obtain an ethyl acetate solution, wherein the initiator comprises dicyclohexyl peroxydicarbonate; S2. The polyester fiber is immersed in m-cresol, washed, and dried, and then placed in the ethyl acetate solution under a protective gas atmosphere for grafting reaction, and then washed and dried to obtain the antibacterial polyester fiber.

2. The preparation method according to claim 1, characterized in that: In step S1, the mass ratio of the wormwood essential oil to the initiator is 1:0.003-0.006; And / or, in the ethyl acetate solution in step S1, the concentration of the wormwood essential oil is 1wt%-3wt%.

3. The preparation method according to claim 1, characterized in that: In step S1, the initiator further includes lauroyl peroxide.

4. The preparation method according to claim 3, characterized in that: In step S1, the mass ratio of lauroyl peroxide to dicyclohexyl peroxydicarbonate is 2-3:4-7.

5. The preparation method according to claim 1, characterized in that: The ethyl acetate solution in step S1 also includes biphenyl.

6. The preparation method according to claim 5, characterized in that: In step S1, the mass ratio of biphenyl to wormwood essential oil is 0.2-0.3:

1.

7. The preparation method according to claim 1, characterized in that: In step S2, the mass ratio of m-cresol to polyester fiber is 10-15:1; And / or, in step S2, the soaking time is 1.5-2.5 hours.

8. The preparation method according to claim 1, characterized in that: In step S2, the temperature of the grafting reaction is 60-80°C, and the duration of the grafting reaction is 1-3 hours.

9. 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° C., and the drying time is 15-25 min.

10. The antibacterial polyester fiber prepared according to the method according to any one of claims 1 to 9.

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