CN119433971A - Antibacterial polyester fiber and preparation method thereof - Google Patents
Antibacterial polyester fiber and preparation method thereof Download PDFInfo
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- CN119433971A CN119433971A CN202411600821.9A CN202411600821A CN119433971A CN 119433971 A CN119433971 A CN 119433971A CN 202411600821 A CN202411600821 A CN 202411600821A CN 119433971 A CN119433971 A CN 119433971A
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- polyester fiber
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- essential oil
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
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 of S1, adding mugwort leaf essential oil and an initiator into ethyl acetate to obtain an ethyl acetate solution, wherein the initiator comprises dicyclohexyl peroxydicarbonate, S2, soaking the polyester fiber in m-cresol, washing and drying, then placing the polyester fiber in the ethyl acetate solution under the atmosphere of protective gas for grafting reaction, and then washing and drying to obtain the antibacterial polyester fiber. According to the invention, substances such as terpineol, caryophyllene oxide and the like with antibacterial effect in the mugwort leaf essential oil are introduced into the polyester fiber in a chemical combination mode, so that the combination strength between the substances such as terpineol, caryophyllene oxide and the like with antibacterial effect and the polyester fiber is improved, and the antibacterial performance durability of the fabric made of the polyester fiber is further improved.
Description
Technical Field
The invention belongs to the technical field of textiles, and particularly relates to an antibacterial polyester fiber and a preparation method thereof.
Background
Polyester fiber commonly called as polyester is a synthetic fiber prepared from polyester raw materials formed by polycondensation of organic dihydric alcohol and aromatic dicarboxylic acid or ester thereof. The polyester fiber has the characteristics of stiff and smooth appearance, good thermal stability (the softening point is 230-240 ℃, the melting point is 255-265 ℃ and the decomposition point is about 300 ℃), high strength (the strength in a dry state is 4-7 cN/dtex), high modulus (the initial modulus can reach 14-17 GPa), moderate extensibility (usually 20-50%), excellent wrinkle resistance and shape retention, excellent elastic recovery performance, wear resistance, light resistance, no sticking hair and the like, and is commonly used in the fields of clothing, bedding, indoor ornaments and the like.
In recent years, with the improvement of living standard, the functions of textiles are not limited to comfort, and more consumers put higher demands on the functions of textiles, such as environmental protection and antibacterial property.
In order to endow the fabric made of polyester fibers with antibacterial effect, an attempt is made to prepare a finishing liquid from an antibacterial agent, and the finishing liquid is adopted to carry out after-finishing on grey fabrics made of polyester fibers. However, the fabric produced by the treatment in this way has poor durability of antibacterial effect, for example, the antibacterial effect is greatly reduced with the increase of the number of washing times.
Disclosure of Invention
Accordingly, the invention aims to provide an antibacterial polyester fiber and a preparation method thereof, which are used for solving the technical problems that the antibacterial effect of the fabric prepared by adopting the finishing liquid to carry out after-finishing on grey cloth made of the polyester fiber is poor in durability and the like.
In order to achieve the above object, the present invention has the following technical scheme:
in a first aspect, the present invention provides a method for preparing an antibacterial polyester fiber, comprising the steps of:
s1, adding mugwort leaf essential oil and an initiator into ethyl acetate to obtain an ethyl acetate solution, wherein the initiator comprises dicyclohexyl peroxydicarbonate;
S2, soaking the polyester fiber in m-cresol, washing and drying, then placing the polyester fiber in the ethyl acetate solution under the atmosphere of protective gas for grafting reaction, and then washing and drying to obtain the antibacterial polyester fiber.
Optionally, in step S1, the mass ratio of the mugwort essential oil to the initiator is 1:0.003-0.006, preferably 1:0.004-0.006.
Optionally, in the ethyl acetate solution in step S1, the concentration of the mugwort leaf essential oil is 1wt% to 3wt%, preferably 1.5wt% to 3wt%.
Optionally, in step S1, the initiator further comprises lauroyl peroxide.
Optionally, in step S1, the mass ratio of lauroyl peroxide to dicyclohexyl peroxydicarbonate is 2-3:4-7, preferably 2.5-3:4-7.
Optionally, the ethyl acetate solution in step S1 further includes biphenyl.
Optionally, in step S1, the mass ratio of biphenyl to mugwort essential oil is 0.2-0.3:1, preferably 0.25-0.3:1.
Optionally, in step S2, the mass ratio of the meta-cresol to the polyester fiber is 10-15:1.
Optionally, in step S2, the soaking period is 1.5-2.5h, preferably 2-2.5h.
Optionally, in step S2, the grafting reaction is carried out at a temperature of 60-80 ℃, preferably 65-80 ℃, and the duration of the grafting reaction is 1-3h, preferably 1.5-3h.
Optionally, in step S2, the mass ratio of the polyester fiber to the ethyl acetate solution is 1:15-20, preferably 1:16-20.
Optionally, in step S2, the temperature of the drying is 50-60 ℃, preferably 55-60 ℃, and the drying time is 15-25min, preferably 20-25min.
The second aspect of the invention also provides an antimicrobial polyester fiber made according to the method described above.
As described above, the antibacterial polyester fiber and the preparation method thereof have the following beneficial effects:
According to the invention, the initiator dicyclohexyl peroxydicarbonate is heated and decomposed to generate free radicals, the free radicals can initiate grafting reaction, and substances such as terpineol, caryophyllene oxide and the like which have antibacterial effects in the mugwort leaf essential oil can be grafted onto the polyester fiber through the grafting reaction, namely, the substances such as terpineol, caryophyllene oxide and the like which have antibacterial effects in the mugwort leaf essential oil are introduced into the polyester fiber through chemical bonding, so that the bonding strength between the substances such as terpineol, caryophyllene oxide and the like which have antibacterial effects in the mugwort leaf essential oil and the polyester fiber is improved, and further the antibacterial performance durability of the fabric made of the polyester fiber is improved.
According to the invention, lauroyl peroxide and dicyclohexyl peroxydicarbonate are compounded for use, so that the grafting efficiency can be improved, more terpineol, caryophyllene oxide and other substances are promoted to be grafted on the polyester fiber, and the antibacterial effect of the fabric made of the polyester fiber is improved.
According to the invention, biphenyl can capture hydrogen radicals on the surface of polyester, so that the stability of the hydrogen radicals is improved, the formation of the polyester radicals is facilitated, the reaction is promoted to proceed in the grafting reaction direction, the grafting rate is improved, and the antibacterial effect of the fabric made of polyester fibers is further improved.
Detailed Description
The present invention will be further described with reference to the following specific examples, but it should be noted that the specific material ratios, process conditions, results, etc. described in the embodiments of the present invention are only for illustrating the present invention, and are not intended to limit the scope of the present invention, and all equivalent changes or modifications according to the spirit of the present invention should be included in the scope of the present invention. In the present invention, "wt%" means mass% unless otherwise specified.
An embodiment of the invention provides a preparation method of an antibacterial polyester fiber, which comprises the following steps:
S1, adding mugwort leaf essential oil and an initiator into ethyl acetate to obtain ethyl acetate solution with mugwort leaf essential oil concentration of 1-3wt%, wherein the mass ratio of mugwort leaf essential oil to the initiator is 1:0.003-0.006, and the initiator comprises dicyclohexyl peroxydicarbonate;
S2, soaking the polyester fiber in 10-15 times of m-cresol for 1.5-2.5 hours, washing and drying, then placing the polyester fiber in 15-20 times of ethyl acetate solution for grafting reaction for 1-3 hours at 60-80 ℃ under the protection gas atmosphere, washing, and drying for 15-25 minutes at 50-60 ℃ to obtain the antibacterial polyester fiber.
In another exemplary embodiment of the present invention, in step S1, the initiator further comprises lauroyl peroxide, the mass ratio of lauroyl peroxide to dicyclohexyl peroxydicarbonate being 2-3:4-7.
In another exemplary embodiment of the present invention, the ethyl acetate solution in step S1 further includes biphenyl, and a mass ratio of biphenyl to mugwort leaf essential oil is 0.2-0.3:1.
Another embodiment of the present invention also provides an antibacterial polyester fiber prepared according to the method as described above.
The present invention will be described in detail with reference to specific exemplary examples. It is also to be understood that the following examples are given solely for the purpose of illustration and are not to be construed as limitations upon the scope of the invention, as many insubstantial modifications and variations are within the scope of the invention as would be apparent to those skilled in the art in light of the foregoing disclosure. The specific process parameters and the like described below are also merely examples of suitable ranges, i.e., one skilled in the art can make a suitable selection from the description herein and are not intended to be limited to the specific values described below.
Example 1
The preparation method of the antibacterial polyester fiber comprises the following specific steps:
S1, adding mugwort leaf essential oil (commercially available) and an initiator dicyclohexyl peroxydicarbonate into ethyl acetate, and uniformly stirring to obtain an ethyl acetate solution with mugwort leaf essential oil concentration of 1wt%, wherein the mass ratio of mugwort leaf essential oil to the initiator dicyclohexyl peroxydicarbonate is 1:0.006;
S2, soaking the polyester fiber in m-cresol with the mass being 15 times of that of the polyester fiber for 2.5 hours, washing the polyester fiber with clear water for 2 times, each time for 4 minutes, airing the polyester fiber, putting the polyester fiber in an ethyl acetate solution (the mass ratio of the polyester fiber to the ethyl acetate solution is 1:15) under the nitrogen gas atmosphere for grafting reaction for 1 hour at the temperature of 80 ℃, washing the polyester fiber with clear water for 2 times, each time for 6 minutes, and drying the polyester fiber at the temperature of 50 ℃ for 25 minutes to obtain the antibacterial polyester fiber.
Example 2
The preparation method of the antibacterial polyester fiber comprises the following specific steps:
s1, adding mugwort leaf essential oil (commercially available) and dicyclohexyl peroxydicarbonate serving as an initiator into ethyl acetate, and uniformly stirring to obtain an ethyl acetate solution with mugwort leaf essential oil concentration of 3wt%, wherein the mass ratio of mugwort leaf essential oil to dicyclohexyl peroxydicarbonate serving as the initiator is 1:0.003;
S2, soaking the polyester fiber in m-cresol with the mass 10 times of that of the polyester fiber for 1.5 hours, washing the polyester fiber with clear water for 3 times, each time for 5 minutes, airing the polyester fiber, putting the polyester fiber in an ethyl acetate solution (the mass ratio of the polyester fiber to the ethyl acetate solution is 1:20) under the nitrogen gas atmosphere for grafting reaction for 3 hours at the temperature of 60 ℃, washing the polyester fiber with clear water for 3 times, each time for 5 minutes, and drying the polyester fiber at the temperature of 60 ℃ for 15 minutes to obtain the antibacterial polyester fiber.
Example 3
The preparation method of the antibacterial polyester fiber comprises the following specific steps:
S1, adding mugwort leaf essential oil (commercially available) and dicyclohexyl peroxydicarbonate serving as an initiator into ethyl acetate, and uniformly stirring to obtain an ethyl acetate solution with mugwort leaf essential oil concentration of 2wt%, wherein the mass ratio of mugwort leaf essential oil to dicyclohexyl peroxydicarbonate serving as the initiator is 1:0.005;
S2, soaking the polyester fiber in m-cresol with the mass of 12 times of that of the polyester fiber for 2 hours, washing the polyester fiber with clear water for 2 times, each time for 5 minutes, airing the polyester fiber, putting the polyester fiber into an ethyl acetate solution (the mass ratio of the polyester fiber to the ethyl acetate solution is 1:18) under the nitrogen gas atmosphere for grafting reaction for 2 hours at the temperature of 70 ℃, washing the polyester fiber with clear water for 3 times, each time for 5 minutes, and drying the polyester fiber at the temperature of 54 ℃ for 20 minutes to obtain the antibacterial polyester fiber.
Example 4
An antibacterial polyester fiber was prepared in the same manner as in example 3 except for the following conditions:
S1, adding mugwort leaf essential oil (commercially available) and an initiator into ethyl acetate, and uniformly stirring to obtain an ethyl acetate solution with mugwort leaf essential oil concentration of 2wt%, wherein the mass ratio of mugwort leaf essential oil to the initiator is 1:0.005, and the initiator consists of lauroyl peroxide and dicyclohexyl peroxydicarbonate according to the mass ratio of 2:7.
Example 5
An antibacterial polyester fiber was prepared in the same manner as in example 3 except for the following conditions:
S1, adding mugwort leaf essential oil (commercially available) and an initiator into ethyl acetate, and uniformly stirring to obtain an ethyl acetate solution with mugwort leaf essential oil concentration of 2wt%, wherein the mass ratio of mugwort leaf essential oil to the initiator is 1:0.005, and the initiator consists of lauroyl peroxide and dicyclohexyl peroxydicarbonate according to the mass ratio of 3:4.
Example 6
An antibacterial polyester fiber was prepared in the same manner as in example 3 except for the following conditions:
S1, adding mugwort leaf essential oil (commercially available), dicyclohexyl peroxydicarbonate serving as an initiator and biphenyl into ethyl acetate, and uniformly stirring to obtain an ethyl acetate solution with mugwort leaf essential oil concentration of 2wt%, wherein the mass ratio of mugwort leaf essential oil to dicyclohexyl peroxydicarbonate serving as the initiator is 1:0.005, and the mass ratio of biphenyl to mugwort leaf essential oil is 0.2:1.
Example 7
An antibacterial polyester fiber was prepared in the same manner as in example 3 except for the following conditions:
S1, adding mugwort leaf essential oil (commercially available), dicyclohexyl peroxydicarbonate serving as an initiator and biphenyl into ethyl acetate, and uniformly stirring to obtain an ethyl acetate solution with mugwort leaf essential oil concentration of 2wt%, wherein the mass ratio of mugwort leaf essential oil to dicyclohexyl peroxydicarbonate serving as the initiator is 1:0.005, and the mass ratio of biphenyl to mugwort leaf essential oil is 0.3:1.
Comparative example 1
The same source polyester fiber as in example 1, which had not been subjected to any treatment.
Antibacterial property detection
The antibacterial polyester fibers prepared in examples 1-7 and the polyester fibers prepared in comparative example 1 are respectively prepared into fabrics, 10cm of samples are taken respectively, antibacterial values of the samples on staphylococcus aureus (ATCC 6538) and escherichia coli (ATCC 1122938) are detected according to an absorption method of evaluation of antibacterial property of textiles of GB/T20944.2-2007, wherein test bacterial solutions are prepared after being cultured according to a culture C method, and the results are shown in Table 1;
Then, each group of samples was machine-washed at room temperature for 10min, at a full water level, at a stirring speed of 180r/min, at a spin-drying speed of 650r/min, at a spin-drying time of 6min, and then naturally air-dried, and after washing-air-dried for 50 times in this cycle, antibacterial values of each sample against Staphylococcus aureus (ATCC 6538) and Escherichia coli (ATCC 1122938) were again measured according to the absorption method, evaluation of antibacterial Properties of textiles of GB/T20944.2-2007, and the results are shown in Table 1.
TABLE 1 antibacterial Property detection results
As can be seen from Table 1, the antibacterial polyester fibers of examples 1 to 7 showed no significant change in antibacterial values against Staphylococcus aureus and Escherichia coli before and after washing. The result shows that in the invention, the initiator dicyclohexyl peroxydicarbonate is heated and decomposed to generate free radicals, the free radicals can initiate grafting reaction, and substances such as terpineol, caryophyllene oxide and the like which have antibacterial effects in the mugwort leaf essential oil can be grafted onto the polyester fiber through the grafting reaction, namely, the substances such as terpineol, caryophyllene oxide and the like which have antibacterial effects in the mugwort leaf essential oil are introduced into the polyester fiber through chemical bonding, so that the bonding strength between the substances such as terpineol, caryophyllene oxide and the like which have antibacterial effects in the mugwort leaf essential oil and the polyester fiber is improved, and further the antibacterial performance durability of the fabric made of the polyester fiber is improved.
As can be seen from table 1, the antibacterial values of the fabrics made of the antibacterial polyester fibers of example 4 and example 5 against staphylococcus aureus and escherichia coli were significantly improved as compared with example 3 with respect to the pre-washing samples. The result shows that the lauroyl peroxide and dicyclohexyl peroxydicarbonate are compounded and used in the invention, so that the grafting efficiency can be improved, more terpineol, caryophyllene oxide and other substances are promoted to be grafted on the polyester fiber, and the antibacterial effect of the fabric made of the polyester fiber is improved.
As can be seen from table 1, the antibacterial polyester fibers of example 6 and example 7 have significantly improved antibacterial values against staphylococcus aureus and escherichia coli compared with example 3 for the pre-washing samples. The result shows that in the invention, biphenyl can capture hydrogen free radical on the surface of polyester, so that the stability of the hydrogen free radical is improved, the formation of the polyester free radical is facilitated, the reaction is promoted to proceed towards the grafting reaction direction, the grafting rate is improved, and the antibacterial effect of the fabric made of polyester fiber is further improved.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (10)
1. The preparation method of the antibacterial polyester fiber is characterized by comprising the following steps of:
s1, adding mugwort leaf essential oil and an initiator into ethyl acetate to obtain an ethyl acetate solution, wherein the initiator comprises dicyclohexyl peroxydicarbonate;
S2, soaking the polyester fiber in m-cresol, washing and drying, then placing the polyester fiber in the ethyl acetate solution under the atmosphere of protective gas for grafting reaction, and then washing and drying to obtain the antibacterial polyester fiber.
2. The preparation method according to claim 1, wherein in the step S1, the mass ratio of the mugwort essential oil to the initiator is 1:0.003-0.006;
and/or, in the ethyl acetate solution in the step S1, the concentration of the mugwort leaf essential oil is 1-3 wt%.
3. The method of claim 1, wherein in step S1, the initiator further comprises lauroyl peroxide.
4. The method according to claim 3, wherein in the step S1, the mass ratio of lauroyl peroxide to dicyclohexyl peroxydicarbonate is 2-3:4-7.
5. The method according to claim 1, wherein the ethyl acetate solution in step S1 further comprises biphenyl.
6. The method according to claim 5, wherein in the step S1, the mass ratio of biphenyl to mugwort essential oil is 0.2-0.3:1.
7. The preparation method according to claim 1, wherein in the step S2, the mass ratio of the m-cresol to the polyester fiber is 10-15:1;
and/or, in the step S2, the soaking time is 1.5-2.5h.
8. The method according to claim 1, wherein in the step S2, the grafting reaction is carried out at a temperature of 60 to 80 ℃ and a duration of 1 to 3 hours.
9. The preparation method according to claim 1, wherein in the step S2, the mass ratio of the polyester fiber to the ethyl acetate solution is 1:15-20;
And/or in the step S2, the temperature of the drying is 50-60 ℃, and the drying time is 15-25min.
10. An antimicrobial polyester fiber made according to the method of any one of claims 1-9.
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CN202411600821.9A CN119433971A (en) | 2024-11-11 | 2024-11-11 | Antibacterial polyester fiber and preparation method thereof |
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CN202411600821.9A CN119433971A (en) | 2024-11-11 | 2024-11-11 | Antibacterial polyester fiber and preparation method thereof |
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