CN115679471A - Preparation method of rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber - Google Patents
Preparation method of rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber Download PDFInfo
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- CN115679471A CN115679471A CN202211577206.1A CN202211577206A CN115679471A CN 115679471 A CN115679471 A CN 115679471A CN 202211577206 A CN202211577206 A CN 202211577206A CN 115679471 A CN115679471 A CN 115679471A
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 86
- 239000000835 fiber Substances 0.000 title claims abstract description 74
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 239000005751 Copper oxide Substances 0.000 title claims abstract description 63
- 229910000431 copper oxide Inorganic materials 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000004952 Polyamide Substances 0.000 title claims abstract description 17
- 229920002647 polyamide Polymers 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 66
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims abstract description 33
- 235000017491 Bambusa tulda Nutrition 0.000 claims abstract description 33
- 241001330002 Bambuseae Species 0.000 claims abstract description 33
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims abstract description 33
- 239000011425 bamboo Substances 0.000 claims abstract description 33
- 239000013081 microcrystal Substances 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 27
- 229920001778 nylon Polymers 0.000 claims abstract description 18
- 238000001125 extrusion Methods 0.000 claims abstract description 7
- 238000005469 granulation Methods 0.000 claims abstract description 7
- 230000003179 granulation Effects 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000004729 solvothermal method Methods 0.000 claims abstract description 3
- 239000000725 suspension Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000004094 surface-active agent Substances 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 8
- 239000004744 fabric Substances 0.000 claims description 8
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 7
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 6
- 238000002074 melt spinning Methods 0.000 claims description 6
- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- 125000002091 cationic group Chemical group 0.000 claims description 4
- 150000001879 copper Chemical class 0.000 claims description 4
- 239000001384 succinic acid Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 125000000129 anionic group Chemical group 0.000 claims description 3
- UCMIRNVEIXFBKS-UHFFFAOYSA-N beta-alanine Chemical compound NCCC(O)=O UCMIRNVEIXFBKS-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 229940075582 sorbic acid Drugs 0.000 claims description 2
- 235000010199 sorbic acid Nutrition 0.000 claims description 2
- 239000004334 sorbic acid Substances 0.000 claims description 2
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 claims 1
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims 1
- 238000009987 spinning Methods 0.000 abstract description 5
- 239000006185 dispersion Substances 0.000 abstract description 3
- 229910052802 copper Inorganic materials 0.000 description 7
- 239000010949 copper Substances 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 241000222122 Candida albicans Species 0.000 description 5
- 241000588724 Escherichia coli Species 0.000 description 5
- 241000191967 Staphylococcus aureus Species 0.000 description 5
- 229940095731 candida albicans Drugs 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 2
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 2
- 230000002045 lasting effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229950000244 sulfanilic acid Drugs 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000002781 deodorant agent Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000011796 hollow space material Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
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Abstract
The invention provides a preparation method of a rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber, which comprises the following specific steps: taking surface modified submicron bamboo fiber microcrystal as a hard template material, preparing multidimensional flaky nano copper oxide to coat the surface of the hard template material by a mixed solvothermal method, and then preparing a rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material by washing, calcining and other methods; the rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material and the PA6 material are subjected to melt extrusion granulation and spinning to prepare rod-shaped hollow nano copper oxide antibacterial wear-resistant nylon fiber; the rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material prepared by the invention has the advantages of small addition amount, light weight, uniform dispersion, good antibacterial wear-resistant performance, stable and durable performance, simple operation and the like when being applied to nylon fibers, and has wide application prospect.
Description
Technical Field
The invention belongs to the field of antibacterial wear-resistant materials and antibacterial wear-resistant fibers, and particularly relates to a preparation method of a rod-shaped hollow nano copper oxide antibacterial wear-resistant nylon fiber.
Background
The nylon fiber has excellent elasticity and rebound resilience, is antistatic, anti-pilling, easy to dye and high in color fastness, so that the nylon fiber has unique advantages incomparable with other chemical fibers in the aspect of blending application, particularly in the field of blending of cotton and chemical fibers, and the fabric made of the nylon fiber is light and soft, has mild skin touch and is widely applied to high-end clothing and special clothing. With the improvement of the living standard of human beings, the market prospect of the antibacterial fiber is wider and wider.
At present, silver-based antibacterial agents are widely adopted as antibacterial aids for antibacterial fibers, however, researches show that silver-containing fibers have certain problems in safety, so that the U.S. natural resource protection committee in 2014 announces that the use of nano silver on textiles is limited. Copper is used as a cheap material, the source is wide, the cost is low, although the antibacterial performance of the copper is slightly inferior to that of silver, the antibacterial and deodorant performance of the copper is lasting and stable, and the copper-rich copper element can also play a role in promoting skin metabolism and improving skin color, so that the copper-based antibacterial nylon fiber is a mainstream variety in the current market.
Disclosure of Invention
The invention aims to provide an antibacterial and wear-resistant double-effect functional material, and a preparation method of polyamide fiber with small addition amount, light weight, uniform dispersion and good antibacterial and wear-resistant properties.
In order to achieve the aim, the invention provides a preparation method of a rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber, which is characterized by comprising the following specific steps:
the first step is as follows: preparing a rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material, wherein the rod-shaped hollow nano copper oxide antibacterial wear-resistant material is prepared by taking surface modified submicron bamboo fiber microcrystals as a hard template material, preparing multidimensional flaky nano copper oxide to coat the surface of the rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material by a mixed solvothermal method, washing, calcining and other methods;
the second step is that: drying and blending the rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material and a PA6 material, performing melt extrusion granulation at 180 to 250 ℃, and finally performing melt spinning to prepare the rod-shaped hollow nano copper oxide antibacterial wear-resistant nylon fiber;
preferably, the preparation method of the surface modified submicron-order bamboo fiber microcrystalline hard template material in the first step comprises the following steps: and (3) dispersing 10-20 g of submicron-order bamboo fiber microcrystal in 100-300mL of distilled water to form a suspension, putting the suspension into an ultrasonic cleaner for dispersion for 10-30min, pouring the suspension into a three-neck flask, adding 0.1-0.5 g of surfactant, putting the mixture into an oil bath at the temperature of 30-50 ℃, and fully stirring and dispersing to obtain the surface modified submicron-order bamboo fiber microcrystal hard template material.
Preferably, the surfactant is at least one of an anionic gemini surfactant, a cationic gemini surfactant and an amphoteric gemini surfactant.
Preferably, the stirring condition is 2000 to 4000r/min.
Preferably, the preparation method of the rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material in the first step comprises the following steps: weighing 0.5-2g of copper salt, 0.5-2g of mineralizer and 1-3g of alkali solution, stirring, adding ethanol water of the surface modified submicron grade bamboo fiber microcrystal hard template material in a certain volume ratio, mixing and dissolving, stirring fully, transferring into a high-pressure reaction kettle, reacting for 24-48h at the temperature of 100-150 ℃, taking out, cooling to room temperature, filtering, washing with deionized water to be neutral, drying the obtained product, and calcining at the temperature of 400-500 ℃ to obtain the rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material.
Preferably, the mass ratio of the surface-modified submicron bamboo fiber microcrystal hard template material to ethanol water is (0.5) - (5); the volume (mL) ratio of the ethanol to the water is 2 to 5 to 8.
Preferably, the copper salt is CuSO 4 ·5H 2 O、Cu(NO 3 ) 2 ·3H 2 O、CuCl 2 ·2H 2 At least one of O.
Preferably, the mineralizer is at least one of sorbic acid, aminopropionic acid, succinic acid and anhydrous sulfanilic acid.
Preferably, the alkali solution is at least one of NaOH, KOH and ammonia.
Preferably, the size of the prepared rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material is 300 to 600nm.
Preferably, the mass ratio of the rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material obtained in the second step to PA6 is 0.05-0.5.
Preferably, the breaking strength (GB/T14344-2008) of the rod-shaped hollow nano copper oxide antibacterial wear-resistant nylon fiber prepared by the technical scheme of the invention is more than or equal to 9 g/denier; the elongation at break (GB/T14344-2008) is more than or equal to 15 percent; the boiling water shrinkage (GB/T6505-2017) is less than or equal to 10 percent; the unevenness rate of strip evenness (GB/T14346-2015) is less than or equal to 2 percent; the wear resistance of a cloth sample woven by the fiber is utilized, and the mass reduction rate (GB/T21196.3-2007) is less than or equal to 0.05 percent.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention adopts the surface modified submicron grade bamboo fiber microcrystal as the hard template material, and utilizes the advantages of abundant hydroxyl on the surface of the bamboo fiber microcrystal, special surface structure with huge specific surface area, abundant sources, low price, easy obtaining, controllable size and shape, easy modification and the like.
(2) The surface modified submicron-level bamboo fiber microcrystal is coated with the nano copper oxide by a chemical method, the multidimensional flaky nano copper oxide is prepared by controlling reaction conditions, and the rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material prepared by high-temperature calcination has a large specific surface area, is an ideal light hollow material, and has a good application prospect.
(3) The antibacterial wear-resistant fiber obtained by the invention has the double-effect functions of antibiosis and wear resistance and has stable performance.
(4) The method has the advantages of simple operation, high efficiency, low cost, lasting effect and wide application prospect.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention can be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the claims appended to the present application.
Example 1
A preparation method of a rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber comprises the following specific steps:
(1) Preparing a surface modified submicron grade bamboo fiber microcrystal hard template material: dispersing 10g of submicron-order bamboo fiber microcrystal in 100mL of distilled water to form a suspension, putting the suspension into an ultrasonic cleaner for dispersing for 10min, pouring the suspension into a three-neck flask, adding 0.1g of anionic gemini surfactant, putting the mixture into an oil bath at 30 ℃, and fully stirring and dispersing at the stirring speed of 2000r/min to obtain a surface modified submicron-order bamboo fiber microcrystal hard template material;
(2) Preparing a rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material: 0.5g of CuSO is weighed and weighed respectively 4 ·5H 2 Adding 0.5g of aminopropionic acid and 1g of a mixed solution of NaOH and KOH (volume ratio is 1;
(3) Preparing the rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber: drying and blending the rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material and the PA6 material according to a mass ratio of 0.05. The breaking strength of the fiber is more than or equal to 9 g/denier; the elongation at break is more than or equal to 15 percent; the boiling water shrinkage is less than or equal to 10 percent; the unevenness rate of the yarn is less than or equal to 2 percent; the antibacterial rate of the fiber to escherichia coli is more than 95%, the antibacterial rate to staphylococcus aureus is more than 90%, the antibacterial rate to candida albicans is more than 65%, and the fabric sample woven by the fiber has the wear-resisting performance and the mass reduction rate of less than or equal to 0.05%.
Example 2
A preparation method of a rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber comprises the following specific steps:
(1) Preparing a surface modified submicron grade bamboo fiber microcrystal hard template material: dispersing 15g of submicron-order bamboo fiber microcrystal in 200mL of distilled water to form a suspension, putting the suspension into an ultrasonic cleaner for dispersing for 20min, pouring the suspension into a three-neck flask, adding 0.3g of cationic gemini surfactant, putting the suspension into an oil bath at 35 ℃, and fully stirring and dispersing at the stirring speed of 2500r/min to obtain a surface modified submicron-order bamboo fiber microcrystal hard template material;
(2) Preparing a rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material: weighing 1.0gCu (NO) separately 3 ) 2 ·3H 2 Adding 1.5g of succinic acid and 2g of ammonia water into a surface modified submicron bamboo fiber microcrystal hard template material ethanol water mixed solution (the volume (mL) ratio is 4);
(3) Preparing the rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber: and (2) drying and blending the rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material and the PA6 material according to a mass ratio of 0.1 to 99.9, performing melt extrusion granulation at 180 to 250 ℃, and finally performing melt spinning (the spinning temperature is 230 to 260 ℃) to prepare the rod-shaped hollow nano copper oxide antibacterial wear-resistant nylon fiber. The breaking strength of the fiber is more than or equal to 10 g/denier; the elongation at break is more than or equal to 20 percent; the boiling water shrinkage is less than or equal to 8 percent; the unevenness rate of the yarn is less than or equal to 1.5 percent; the antibacterial rate of the fiber to escherichia coli is more than 98%, the antibacterial rate to staphylococcus aureus is more than 92%, the antibacterial rate to candida albicans is more than 73%, and the fabric sample woven by the fiber has the wear-resisting performance and the mass reduction rate of less than or equal to 0.03%.
Example 3
A preparation method of a rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber comprises the following specific steps:
(1) Preparing a surface modified submicron grade bamboo fiber microcrystal hard template material: dispersing 18g of submicron-order bamboo fiber microcrystal in 300mL of distilled water to form a suspension, putting the suspension into an ultrasonic cleaner for dispersing for 30min, pouring the suspension into a three-neck flask, adding 0.35g of amphoteric gemini surfactant, putting the mixture into an oil bath at 40 ℃, and fully stirring and dispersing at the stirring speed of 3000r/min to obtain a surface modified submicron-order bamboo fiber microcrystal hard template material;
(2) Preparing a rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material: 2g of CuCl were weighed out separately 2 ·2H 2 Adding 1.5g of anhydrous sulfanilic acid and 2g of NaOH into a surface modified submicron bamboo fiber microcrystalline hard template material ethanol-water mixed solution (the volume (mL) ratio is 2);
(3) Preparing the rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber: drying and blending the rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material and the PA6 material according to a mass ratio of 0.15 to 99.85, performing melt extrusion granulation at 180 to 250 ℃, and finally performing melt spinning (the spinning temperature is 230 to 260 ℃) to prepare the rod-shaped hollow nano copper oxide antibacterial wear-resistant nylon fiber. The breaking strength of the fiber is more than or equal to 11 g/denier; the elongation at break is more than or equal to 13 percent; the boiling water shrinkage is less than or equal to 20 percent; the unevenness rate of the yarn is less than or equal to 2.5 percent; the antibacterial rate of the fiber to escherichia coli is more than 98%, the antibacterial rate to staphylococcus aureus is more than 94%, the antibacterial rate to candida albicans is more than 75%, and the fabric sample woven by the fiber has the wear-resisting performance, and the mass reduction rate is less than or equal to 0.02%.
Example 4
A preparation method of a rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber comprises the following specific steps:
(1) Preparing a surface modified submicron grade bamboo fiber microcrystal hard template material: dispersing 20g of submicron-order bamboo fiber microcrystal in 250mL of distilled water to form a suspension, putting the suspension into an ultrasonic cleaner for dispersing for 30min, pouring the suspension into a three-neck flask, adding 0.3g of cationic gemini surfactant, putting the suspension into an oil bath at 45 ℃, and fully stirring and dispersing at a stirring speed of 3500r/min to obtain a surface modified submicron-order bamboo fiber microcrystal hard template material;
(2) Preparing a rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material: weighing 1.5g of CuSO respectively 4 ·5H 2 Adding a mixed solution (volume ratio is 1;
(3) Preparing the rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber: and (2) drying the rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material and the PA6 material according to a mass ratio of 0.25 to 99.75, blending, performing melt extrusion granulation at 180 to 250 ℃, and finally performing melt spinning (the spinning temperature is 230 to 260 ℃) to prepare the rod-shaped hollow nano copper oxide antibacterial wear-resistant nylon fiber. The breaking strength of the fiber is more than or equal to 13 g/denier; the elongation at break is more than or equal to 9 percent; the boiling water shrinkage is less than or equal to 25 percent; the unevenness rate of the yarn is less than or equal to 3 percent; the antibacterial rate of the fiber to escherichia coli is more than 99%, the antibacterial rate to staphylococcus aureus is more than 96%, the antibacterial rate to candida albicans is more than 83%, and the fabric sample woven by the fiber has the wear-resisting property and the mass reduction rate of less than or equal to 0.01%.
Example 5
A preparation method of a rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber comprises the following specific steps:
(1) Preparing a surface modified submicron grade bamboo fiber microcrystal hard template material: dispersing 12g of submicron-order bamboo fiber microcrystal in 120mL of distilled water to form a suspension, putting the suspension into an ultrasonic cleaner for dispersing for 15min, pouring the suspension into a three-neck flask, adding 0.15g of a double-ion gemini surfactant, putting the mixture into an oil bath at 40 ℃, and fully stirring and dispersing at the stirring speed of 2500r/min to obtain a surface modified submicron-order bamboo fiber microcrystal hard template material;
(2) Preparing a rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material: 0.75gCu (NO) was weighed out separately 3 ) 2 ·3H 2 Adding a mixed solution of O, 0.75g of succinic acid and 1.5g of KOH (volume ratio is 2;
(3) Preparing the rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber: and (2) drying the rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material and the PA6 material according to a mass ratio of 0.35 to 99.65, blending, performing melt extrusion granulation at 180 to 250 ℃, and finally performing melt spinning (the spinning temperature is 230 to 260 ℃) to prepare the rod-shaped hollow nano copper oxide antibacterial wear-resistant nylon fiber. The breaking strength of the fiber is more than or equal to 10 g/denier; the elongation at break is more than or equal to 12 percent; the boiling water shrinkage is less than or equal to 8.5 percent; the unevenness rate of the yarn is less than or equal to 2.5 percent; the antibacterial rate of the fiber to escherichia coli is more than 93%, the antibacterial rate to staphylococcus aureus is more than 88%, the antibacterial rate to candida albicans is more than 63%, and the wear-resisting property of a cloth sample woven by the fiber is that the mass reduction rate is less than or equal to 0.04%.
The foregoing description has described specific embodiments of the present invention. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (5)
1. A preparation method of a rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber is characterized by comprising the following specific steps:
the first step is as follows: preparing a rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material, wherein the rod-shaped hollow nano copper oxide antibacterial wear-resistant material is prepared by taking surface modified submicron bamboo fiber microcrystals as a hard template material, preparing multidimensional flaky nano copper oxide to coat the surface of the rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material by a mixed solvothermal method, washing, calcining and other methods;
the second step: and (2) drying and blending the rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material and a PA6 material, performing melt extrusion granulation at 180 to 250 ℃, and finally performing melt spinning to prepare the rod-shaped hollow nano copper oxide antibacterial wear-resistant nylon fiber.
2. The preparation method of the rod-shaped hollow nano copper oxide antibacterial wear-resistant nylon fiber according to claim 1, wherein the preparation method of the surface modified submicron bamboo fiber microcrystalline hard template material in the first step comprises the following steps: dispersing 10-20 g of submicron-order bamboo fiber microcrystal in 100-300mL of distilled water to form a suspension, putting the suspension into an ultrasonic cleaner, dispersing for 10-30min, pouring the suspension into a three-neck flask, adding 0.1-0.5 g of surfactant, putting the suspension into an oil bath at the temperature of 30-50 ℃, and fully stirring and dispersing to obtain a surface modified submicron-order bamboo fiber microcrystal hard template material;
the surfactant is at least one of an anionic gemini surfactant, a cationic gemini surfactant and an amphoteric gemini surfactant;
the stirring condition is 2000 to 4000r/min.
3. The preparation method of the rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber according to claim 1, wherein the preparation method of the rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material in the first step comprises the following steps: weighing 0.5 to 2g of copper salt, 0.5 to 2g of mineralizer and 1 to 3g of alkali solution, stirring, adding ethanol water of the surface modified submicron grade bamboo fiber microcrystal hard template material in a certain volume ratio, mixing and dissolving, stirring fully, transferring into a high-pressure reaction kettle, reacting for 24 to 48h at the temperature of 100 to 150 ℃, taking out, cooling to room temperature, filtering, washing with deionized water to be neutral, drying the obtained product, and calcining at the temperature of 400 to 500 ℃ to obtain the rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material;
the mass ratio of the surface-modified submicron bamboo fiber microcrystal hard template material to the ethanol water is (0.5) - (5); the volume (mL) ratio of the ethanol to the water is 2 to 5 to 8;
the copper salt is at least one of CuSO4.5H2O, cu (NO 3) 2.3H2O and CuCl2.2H2O;
the mineralizer is at least one of sorbic acid, aminopropionic acid, succinic acid and anhydrous sulfanilic acid;
the alkali solution is at least one of NaOH, KOH and ammonia water;
the size of the prepared rod-shaped hollow nano copper oxide antibacterial wear-resistant powder material is 300 to 600nm.
4. The preparation method of the antibacterial and wear-resistant rod-shaped hollow nano copper oxide nylon fiber according to claim 1, wherein the mass ratio of the antibacterial and wear-resistant rod-shaped hollow nano copper oxide powder material obtained in the second step to PA6 is (0.05) - (0.5) - (99.5) - (99.95).
5. The preparation method of the rod-shaped hollow nano copper oxide antibacterial wear-resistant nylon fiber according to claim 1, wherein the breaking strength (GB/T14344-2008) of the rod-shaped hollow nano copper oxide antibacterial wear-resistant nylon fiber is not less than 9 g/denier; the elongation at break (GB/T14344-2008) is more than or equal to 15 percent; the boiling water shrinkage (GB/T6505-2017) is less than or equal to 10 percent; the unevenness rate of strip dryness (GB/T14346-2015) is less than or equal to 2 percent; the wear resistance of the cloth sample woven by the fiber has the mass reduction rate (GB/T21196.3-2007) less than or equal to 0.05 percent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211577206.1A CN115679471A (en) | 2022-12-09 | 2022-12-09 | Preparation method of rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211577206.1A CN115679471A (en) | 2022-12-09 | 2022-12-09 | Preparation method of rod-shaped hollow nano copper oxide antibacterial wear-resistant polyamide fiber |
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