CN116442615A - Cool antibacterial fabric containing inorganic composite nylon, and preparation method and application thereof - Google Patents
Cool antibacterial fabric containing inorganic composite nylon, and preparation method and application thereof Download PDFInfo
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- CN116442615A CN116442615A CN202310702855.8A CN202310702855A CN116442615A CN 116442615 A CN116442615 A CN 116442615A CN 202310702855 A CN202310702855 A CN 202310702855A CN 116442615 A CN116442615 A CN 116442615A
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- CN
- China
- Prior art keywords
- graphene oxide
- nylon
- inorganic composite
- boron nitride
- hexagonal boron
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- 239000004744 fabric Substances 0.000 title claims abstract description 139
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 69
- 229920001778 nylon Polymers 0.000 title claims abstract description 62
- 239000004677 Nylon Substances 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 149
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 121
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229910052582 BN Inorganic materials 0.000 claims abstract description 68
- 239000000835 fiber Substances 0.000 claims abstract description 56
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 29
- 229920001661 Chitosan Polymers 0.000 claims abstract description 27
- 239000004593 Epoxy Substances 0.000 claims abstract description 26
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims abstract description 25
- 235000017491 Bambusa tulda Nutrition 0.000 claims abstract description 25
- 241001330002 Bambuseae Species 0.000 claims abstract description 25
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims abstract description 25
- 239000011425 bamboo Substances 0.000 claims abstract description 25
- 229920000742 Cotton Polymers 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 241000722949 Apocynum Species 0.000 claims abstract description 13
- 229920000728 polyester Polymers 0.000 claims abstract description 13
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 10
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002074 melt spinning Methods 0.000 claims abstract description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 156
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 60
- 238000009940 knitting Methods 0.000 claims description 60
- 238000006243 chemical reaction Methods 0.000 claims description 59
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 54
- 238000001035 drying Methods 0.000 claims description 54
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 238000005406 washing Methods 0.000 claims description 42
- 238000003756 stirring Methods 0.000 claims description 41
- DBGVGMSCBYYSLD-UHFFFAOYSA-N tributylstannane Chemical compound CCCC[SnH](CCCC)CCCC DBGVGMSCBYYSLD-UHFFFAOYSA-N 0.000 claims description 34
- 238000001914 filtration Methods 0.000 claims description 33
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 32
- 239000007864 aqueous solution Substances 0.000 claims description 32
- 150000001263 acyl chlorides Chemical class 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 22
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000009941 weaving Methods 0.000 claims description 21
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 20
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- 229960000583 acetic acid Drugs 0.000 claims description 16
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- 238000001132 ultrasonic dispersion Methods 0.000 claims description 15
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- 239000007788 liquid Substances 0.000 claims description 12
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 10
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 claims description 9
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- 238000009987 spinning Methods 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 2
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- 229920006052 Chinlon® Polymers 0.000 claims 2
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- 238000012986 modification Methods 0.000 abstract description 4
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- 229920002292 Nylon 6 Polymers 0.000 description 8
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- 239000012299 nitrogen atmosphere Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 239000011159 matrix material Substances 0.000 description 6
- 230000007935 neutral effect Effects 0.000 description 6
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- 239000002262 Schiff base Substances 0.000 description 4
- 150000004753 Schiff bases Chemical class 0.000 description 4
- 230000003385 bacteriostatic effect Effects 0.000 description 4
- 230000006870 function Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000004814 polyurethane Substances 0.000 description 4
- 229920002635 polyurethane Polymers 0.000 description 4
- 239000004900 Hydrophilic Finishing Agent Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 210000004243 sweat Anatomy 0.000 description 3
- 241000588724 Escherichia coli Species 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 125000003172 aldehyde group Chemical group 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 1
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
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- 150000001412 amines Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 235000009120 camo Nutrition 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 235000005607 chanvre indien Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
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- 238000005260 corrosion Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
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- 239000007769 metal material Substances 0.000 description 1
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- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
- B32B5/08—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer the fibres or filaments of a layer being of different substances, e.g. conjugate fibres, mixture of different fibres
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/30—Antimicrobial, e.g. antibacterial
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
- B32B5/026—Knitted fabric
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
- B32B5/06—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer characterised by a fibrous or filamentary layer mechanically connected, e.g. by needling to another layer, e.g. of fibres, of paper
- B32B5/073—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer characterised by a fibrous or filamentary layer mechanically connected, e.g. by needling to another layer, e.g. of fibres, of paper characterised by the fibrous or filamentary layer being mechanically connected to another layer by sewing, stitching, hook-and-loop fastening or stitchbonding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
- B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
- B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B2038/0052—Other operations not otherwise provided for
- B32B2038/008—Sewing, stitching
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/02—Synthetic macromolecular fibres
- B32B2262/0261—Polyamide fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/02—Synthetic macromolecular fibres
- B32B2262/0276—Polyester fibres
- B32B2262/0284—Polyethylene terephthalate [PET] or polybutylene terephthalate [PBT]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/06—Vegetal fibres
- B32B2262/062—Cellulose fibres, e.g. cotton
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/06—Vegetal fibres
- B32B2262/062—Cellulose fibres, e.g. cotton
- B32B2262/065—Lignocellulosic fibres, e.g. jute, sisal, hemp, flax, bamboo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/14—Mixture of at least two fibres made of different materials
- B32B2262/152—Knitted fabric
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/306—Resistant to heat
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
- B32B2307/7145—Rot proof, resistant to bacteria, mildew, mould, fungi
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention belongs to the field of textile processing, and discloses a cool antibacterial fabric containing inorganic composite nylon, and a preparation method and application thereof. The preparation method comprises the following steps: reacting the aldehyde graphene oxide with chitosan to obtain modified graphene oxide; after hydroxylation modification, the hexagonal boron nitride reacts with epoxypropyl trimethoxy silane to obtain epoxy modified hexagonal boron nitride; reacting the modified graphene oxide with epoxy modified hexagonal boron nitride to obtain cool antibacterial functional powder; mixing the cool antibacterial functional powder with nylon master batch, melt spinning, and chopping to obtain modified nylon fiber; the inner layer fabric is prepared by taking modified nylon fibers, cotton fibers and bamboo fibers as raw materials, the outer layer fabric is prepared by taking polyester fibers, bamboo fibers and apocynum fibers as raw materials, and the inner layer fabric and the outer layer fabric are sewed to prepare the cool antibacterial fabric containing inorganic composite nylon. The fabric is soft and has excellent antibacterial property and lasting cooling feeling.
Description
Technical Field
The invention belongs to the field of textile processing, and particularly relates to a preparation method of a cool antibacterial fabric containing inorganic composite nylon.
Background
Along with the economic development, textile fabrics are updated, and some high polymer materials are endowed with functionality to enter the textile field, so that the requirements of people on the fabrics are met. In summer, when the human body is easy to sweat to form a high-temperature and high-humidity environment and sweat cannot be discharged in time, bacteria are easy to breed, and discomfort is caused. Therefore, people are required to have comfortable and quick-drying performances and cool and antibacterial performances on summer clothing, including body-building clothing, sun-proof clothing and the like. In the prior art, some natural fibers, such as silk fibers, wool fibers, cotton fibers, hemp fibers, etc., exhibit good breathability and comfort, but are generally bacteriostatic. The nylon is used as a common fabric in the field of textile processing, has strong comprehensive advantages, is skin-friendly and moisture-absorbing, has higher wear resistance than all other fibers, is quick-drying and sun-proof, has low cost, and meets the basic requirements of people in the current society on the fabric. In the prior art, some cool sense substances with slow release function effectively combine with clothes by releasing cool sense factors, so as to prolong the duration of cool sense effect. In the actual use process, the single cool sense finishing is not enough to relieve the problem that the fabric is sweated in high wet weather or a large amount of sweat, and further improvement is needed.
Chinese patent CN109736078B discloses a finishing process of moisture-absorbing cool sportswear fabric, which obtains hexagonal boron nitride nanosheets by nano boron nitride powder treatment; mixing hexagonal boron nitride nanosheets, hydrophilic finishing agents and titanate coupling agents to prepare dispersion finishing liquid; alkali modification treatment is carried out on the polyester-polyurethane fabric; padding the treated alkali modified polyester-polyurethane fabric in the dispersion finishing liquid, performing secondary padding and secondary padding, pre-drying, and baking to obtain the moisture-absorbing cool polyester-polyurethane sportswear fabric. The fabric is subjected to moisture absorption and cooling function finishing by adopting a padding method, the cooling feeling of the fabric can be realized by the hydroxylated nano BN powder contained in the dispersion finishing liquid, the moisture absorption of the fabric can be increased by the hydrophilic finishing agent, but the moisture absorption and cooling performance of the fabric can be continuously weakened along with gradual falling off of the hydroxylated nano boron nitride powder and the hydrophilic finishing agent from the surface of the fabric along with the increase of the service time and the washing times, and the antibacterial performance of the polyester-polyurethane fabric is not improved, so that the antibacterial function cannot be achieved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a cool antibacterial fabric containing inorganic composite nylon. The cool antibacterial fabric containing the inorganic composite nylon, which is prepared by the preparation method, has excellent antibacterial performance and lasting cool feeling.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a cool antibacterial fabric containing inorganic composite nylon comprises the following steps:
preparing graphene oxide into graphene oxide dispersion liquid by deionized water, adding HBr aqueous solution, reacting, adding oxalic acid, continuing the reaction, centrifuging, washing and drying to obtain carboxylated graphene oxide; mixing carboxylated graphene oxide and thionyl chloride, performing ultrasonic dispersion, reacting, and performing reduced pressure distillation to obtain acyl chloride graphene oxide;
step (2) adding acyl chloride graphene oxide into ethyl acetate, dropwise adding ethyl acetate solution of tri-n-butyl tin hydride, stirring, reacting, filtering after the reaction, and drying to obtain aldehyde graphene oxide;
step (3) adding chitosan and aldehyde graphene oxide into ethanol, adding glacial acetic acid, reacting, filtering, washing and drying to obtain modified graphene oxide;
step (4) mixing epoxy modified hexagonal boron nitride, modified graphene oxide, tetrahydrofuran and N-methyldiethanolamine, reacting, filtering, washing and drying to obtain cool antibacterial functional powder;
step (5) mixing the cool antibacterial functional powder with nylon master batch, and spinning to obtain modified nylon fiber;
step (6), spinning the inner layer raw material to obtain an inner layer fabric; weaving the outer layer raw materials to obtain an outer layer fabric; after the inner layer fabric and the outer layer fabric are aligned and overlapped, stitching to obtain the cool antibacterial fabric containing the inorganic composite nylon; wherein the inner layer raw material comprises modified nylon fiber, cotton fiber and bamboo fiber; the outer layer raw materials comprise polyester fiber, bamboo fiber and apocynum fiber.
Preferably, in the step (1): when preparing carboxylated graphene oxide, the mass ratio of graphene oxide, HBr aqueous solution and oxalic acid is 0.075:7.45:1.5, the reaction condition is stirring and reacting for 12 hours at room temperature, and the continuous reaction condition is stirring and reacting for 4 hours at room temperature; when preparing the acyl chloride graphene oxide, the mass ratio of carboxylated graphene oxide to thionyl chloride is (20-40): (4000-8000) under the reaction condition of 65-75 ℃ for 24-40h.
Preferably, in the step (2), the mass ratio of the ethyl acetate solution of the acyl chloride graphene oxide, the ethyl acetate and the tri-n-butyl tin hydride is (20-30): (200-600): (270-310), the dripping condition of the ethyl acetate solution of the tri-n-butyl tin hydride is that the reaction is carried out for 13-15h at room temperature in 0 ℃ and inert gas atmosphere.
Preferably, in the step (3), the reaction conditions are that the reaction is carried out at a temperature of 60-80 ℃ for 2-6 hours.
Preferably, in the step (4), the mass ratio of epoxy modified hexagonal boron nitride, modified graphene oxide, tetrahydrofuran and N-methyldiethanolamine is (80-100): (60-80): (3000-5000): (10-22).
Preferably, the epoxy modified hexagonal boron nitride in the step (4) is prepared by the following steps:
adding hexagonal boron nitride into a sodium hydroxide aqueous solution, performing ultrasonic dispersion, stirring for reaction, cooling, performing suction filtration, washing and drying to obtain hydroxylated hexagonal boron nitride; mixing ethanol, hydroxylated hexagonal boron nitride and epoxypropyl trimethoxy silane, reacting, filtering, washing and drying to obtain the epoxy modified hexagonal boron nitride.
Preferably, the spinning in the step (5) comprises melt spinning and chopping after the melt spinning.
Preferably, in the step (6), the modified nylon fiber, the cotton fiber and the bamboo fiber are blended to prepare an inner layer yarn, and then the inner layer yarn is knitted and woven by using a weft knitting circular knitting machine to obtain an inner layer fabric; blending polyester fiber, bamboo fiber and apocynum fiber to obtain outer layer yarns, and knitting and weaving the outer layer yarns by using a weft knitting circular knitting machine to obtain outer layer fabrics; and (3) after the inner layer fabric and the outer layer fabric are aligned and overlapped, stitching to obtain the cool antibacterial fabric containing the inorganic composite nylon.
Preferably, the cool antibacterial fabric containing the inorganic composite nylon is prepared by the preparation method of the cool antibacterial fabric containing the inorganic composite nylon.
Preferably, the cool antibacterial fabric containing the inorganic composite nylon is applied to clothes.
Compared with the prior art, the invention has the beneficial effects that: the graphene oxide disclosed by the invention can cut cell membranes of bacteria, effectively kills the bacteria, has excellent antibacterial property, effectively avoids aggregation of graphene oxide after being modified, can be better dispersed into a nylon master batch base material, improves dispersibility, is convenient for forming a heat-conducting network transmission path, and improves the cooling sensation of the fabric. The chitosan is used as an organic antibacterial agent and has antibacterial property, and active groups including hydroxyl and amino are contained on the chitosan. Chitosan reacts with aldehyde graphene oxide, and amine (-NH) groups on chitosan molecules 2 ) The aldehyde group reacts with active carbonyl (-C=O-) in aldehyde group on aldehyde graphene oxide molecular chain to generate a new group carbon-nitrogen double bond (-C=N-), namely Schiff base, which has inhibition effect on various harmful bacteria, in particular to escherichia coli,Staphylococcus aureus has good inhibiting effect. Therefore, when the antibacterial substance chitosan is introduced, a new antibacterial group is generated through reaction, and the antibacterial performance is improved.
According to the invention, the hexagonal boron nitride has a honeycomb structure similar to graphene, has high hydrophobicity, high thermal conductivity, high temperature stability, acid and alkali corrosion resistance, good processing performance, no toxicity and environmental protection, is compounded with nano materials after being modified by epoxypropyl trimethoxy silane, has excellent characteristics, increases the dispersibility in a matrix, enhances the interfacial compatibility between the matrix and a polymer matrix, and forms a continuous heat conducting particle passage by mutually overlapping the matrix and the graphene oxide, and heat is mainly transferred along a heat conducting network to improve the thermal conductivity of nylon fibers through synergistic effect. Meanwhile, epoxy groups in the epoxy modified hexagonal boron nitride can react with active groups such as amino groups in the modified graphene oxide, and the epoxy groups and the active groups are connected through chemical bonds, so that stability is improved.
The nylon provided by the invention has the characteristics of quick drying, and simultaneously has good heat resistance and plasticity, and bacteria are not easy to generate. The inner layer fabric has excellent antibacterial performance and mechanical property, and improves the comfort degree after weaving; the outer layer fabric is woven by polyester fibers, bamboo fibers and apocynum fibers, and has good ventilation and moisture-conducting functions; the fabric is comfortable after weaving.
Drawings
FIG. 1 is a flow chart of the invention for preparing a cool antibacterial fabric containing inorganic composite nylon;
FIG. 2 is a flow chart of the preparation of modified graphene oxide of the present invention;
FIG. 3 is a flow chart of the preparation of the cool and antibacterial functional powder of the present invention;
FIG. 4 is a schematic reaction diagram of the present invention aldehyde-modified graphene oxide grafted chitosan.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by those skilled in the art without making any inventive effort based on the embodiments of the present invention are within the scope of protection of the present invention.
Example 1
Preparing graphene oxide into 2.5mg/mL graphene oxide dispersion liquid by deionized water, adding 5mLHBr aqueous solution (the mass percentage of HBr is 47%), reacting for 12 hours at the stirring speed of 1000r/min and the room temperature environment, adding oxalic acid, and continuing to react for 4 hours at the stirring speed of 1000r/min and the room temperature environment, wherein the mass ratio of graphene oxide, HBr aqueous solution and oxalic acid is 0.075:7.45:1.5, centrifuging for 5min at a rotating speed of 10000r/min after the reaction, taking a precipitate, washing the precipitate with deionized water for 3 times, and drying for 4h at a temperature of 40 ℃ to obtain carboxylated graphene oxide; the mass ratio is 20: mixing 4000 carboxylated graphene oxide and thionyl chloride, performing ultrasonic dispersion at a frequency of 20kHz for 50min, reacting at 65 ℃ for 40h, and performing reduced pressure distillation at 0.08MPa after the reaction to obtain acyl chloride graphene oxide;
step (2) adding acyl chloride graphene oxide into ethyl acetate, and dropwise adding an ethyl acetate solution of tri-n-butyl tin hydride at the temperature of 0 ℃ in a nitrogen atmosphere, wherein the mass ratio of the acyl chloride graphene oxide to the ethyl acetate solution of the ethyl acetate to the tri-n-butyl tin hydride is 20:200:270, the ethyl acetate solution of the tri-n-butyl tin hydride is prepared from the tri-n-butyl tin hydride and ethyl acetate according to the mass ratio of 40:230, stirring for 30min at the temperature of 0 ℃, heating to room temperature, maintaining the room temperature for reaction for 15h, filtering after the reaction, and drying for 3h at the temperature of 80 ℃ to obtain the aldehyde graphene oxide;
step (3) adding chitosan and aldehyde graphene oxide into ethanol, adding glacial acetic acid, and reacting for 6 hours at the temperature of 60 ℃, wherein the mass ratio of the aldehyde graphene oxide to the ethanol to the chitosan to the glacial acetic acid is 100:1400:200:80, after the reaction, filtering, washing and drying for 3 hours at the temperature of 80 ℃ to obtain modified graphene oxide;
step (4) adding hexagonal boron nitride into 5mol/L sodium hydroxide aqueous solution, wherein the mass ratio of the hexagonal boron nitride to the sodium hydroxide aqueous solution is 1:50, performing ultrasonic dispersion for 60min at the frequency of 20kHz, stirring for 14h at the temperature of 60 ℃ at the stirring speed of 1600r/min, cooling to room temperature, performing suction filtration, washing filter residues with deionized water until the filter residues are neutral, and drying at 60 ℃ for 36h to obtain hydroxylated hexagonal boron nitride; ethanol, hydroxylated hexagonal boron nitride and epoxypropyl trimethoxy silane are mixed according to the mass ratio of 3000:100:40, reacting for 12 hours at 100 ℃, filtering after the reaction, washing filter residues by using ethanol, and drying for 12 hours at 80 ℃ to obtain epoxy modified hexagonal boron nitride;
step (5) epoxy modified hexagonal boron nitride, modified graphene oxide, tetrahydrofuran and N-methyldiethanolamine according to the mass ratio of 80:60:3000:10, mixing, reacting for 8 hours at the temperature of 100 ℃, filtering, washing, and drying for 8 hours at the temperature of 60 ℃ to obtain cool and antibacterial functional powder;
step (6) the mass ratio is 5:80 and nylon 6 master batch are mixed, melt-spun at 230 ℃ and chopped to obtain modified nylon fibers;
step (7) modified nylon fiber, cotton fiber and bamboo fiber according to the mass ratio of 1:1:1, and then knitting and weaving the inner layer yarns by using a weft knitting circular knitting machine to obtain the inner layer fabric, wherein the English count of the inner layer yarns is 45s, and the gram weight of the inner layer fabric is 250g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the Polyester fiber, bamboo fiber and apocynum fiber according to the mass ratio of 1:1:1, and then knitting and weaving the outer layer yarns by using a knitting weft knitting circular knitting machine to obtain an outer layer fabric, wherein the English count of the outer layer yarns is 45s, and the gram weight of the outer layer fabric is 250g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the And after the inner layer fabric and the outer layer fabric are aligned and laminated, sewing the shaped inner layer fabric and the shaped outer layer fabric by using a pure cotton sewing thread with the English count of 40s through a multi-layer fabric quilting machine to obtain the cool antibacterial fabric containing the inorganic composite nylon.
Example 2
Preparing graphene oxide into 2.5mg/mL graphene oxide dispersion liquid by deionized water, adding 5mLHBr aqueous solution (the mass percentage of HBr is 47%), reacting for 12 hours at the stirring speed of 1000r/min and the room temperature environment, adding oxalic acid, and continuing to react for 4 hours at the stirring speed of 1000r/min and the room temperature environment, wherein the mass ratio of graphene oxide, HBr aqueous solution and oxalic acid is 0.075:7.45:1.5, centrifuging for 5min at a rotating speed of 10000r/min after the reaction, taking a precipitate, washing the precipitate with deionized water for 3 times, and drying for 4h at a temperature of 40 ℃ to obtain carboxylated graphene oxide; the mass ratio is 25:5000 carboxylated graphene oxide and thionyl chloride are mixed, dispersed for 45min under the frequency of 25kHz, reacted for 36h at the temperature of 67.5 ℃, and distilled under reduced pressure under the pressure of 0.08MPa after the reaction, so as to obtain acyl chloride graphene oxide;
step (2) adding acyl chloride graphene oxide into ethyl acetate, and dropwise adding an ethyl acetate solution of tri-n-butyl tin hydride at the temperature of 0 ℃ in a nitrogen atmosphere, wherein the mass ratio of the acyl chloride graphene oxide to the ethyl acetate solution of the ethyl acetate to the tri-n-butyl tin hydride is 22.5:300:275, the ethyl acetate solution of tri-n-butyltin hydride is prepared from tri-n-butyltin hydride and ethyl acetate according to a mass ratio of 45:230, stirring for 30min at the temperature of 0 ℃, heating to room temperature, keeping the room temperature for 14.5h, filtering after the reaction, and drying for 2.5h at the temperature of 85 ℃ to obtain the aldehyde graphene oxide;
step (3) adding chitosan and aldehyde graphene oxide into ethanol, adding glacial acetic acid, and reacting for 5 hours at the temperature of 65 ℃, wherein the mass ratio of the aldehyde graphene oxide to the ethanol to the chitosan to the glacial acetic acid is 125:1650:250:85, filtering, washing and drying for 2.5 hours at the temperature of 85 ℃ after the reaction to obtain modified graphene oxide;
step (4) adding hexagonal boron nitride into 5mol/L sodium hydroxide aqueous solution, wherein the mass ratio of the hexagonal boron nitride to the sodium hydroxide aqueous solution is 1:55, performing ultrasonic dispersion for 55min at a frequency of 25kHz, stirring at a stirring speed of 1900r/min and a temperature of 65 ℃ for 13h, cooling to room temperature, performing suction filtration, washing filter residues with deionized water until the filter residues are neutral, and drying at 65 ℃ for 33h to obtain hydroxylated hexagonal boron nitride; ethanol, hydroxylated hexagonal boron nitride and epoxypropyl trimethoxysilane are mixed according to the mass ratio of 3625:100:45, reacting for 11 hours at 105 ℃, filtering after the reaction, washing filter residues by using ethanol, and drying for 11 hours at 85 ℃ to obtain epoxy modified hexagonal boron nitride;
step (5) epoxy modified hexagonal boron nitride, modified graphene oxide, tetrahydrofuran and N-methyldiethanolamine according to a mass ratio of 85:65:3500:13, mixing, reacting for 7 hours at 105 ℃, filtering, washing, and drying for 7.5 hours at 65 ℃ to obtain cool and antibacterial functional powder;
and (6) mixing the materials with the mass ratio of 6:85 and nylon 6 master batch are mixed, melt-spun at 230 ℃, and chopped to obtain modified nylon fibers;
step (7) modified nylon fiber, cotton fiber and bamboo fiber according to the mass ratio of 2:1:1, and then knitting and weaving the inner layer yarns by using a weft knitting circular knitting machine to obtain the inner layer fabric, wherein the English count of the inner layer yarns is 45s, and the gram weight of the inner layer fabric is 250g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the Polyester fiber, bamboo fiber and apocynum fiber according to the mass ratio of 3:1:1, and then knitting and weaving the outer layer yarns by using a knitting weft knitting circular knitting machine to obtain an outer layer fabric, wherein the English count of the outer layer yarns is 45s, and the gram weight of the outer layer fabric is 250g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the And after the inner layer fabric and the outer layer fabric are aligned and laminated, sewing the shaped inner layer fabric and the shaped outer layer fabric by using a pure cotton sewing thread with the English count of 40s through a multi-layer fabric quilting machine to obtain the cool antibacterial fabric containing the inorganic composite nylon.
Example 3
Preparing graphene oxide into 2.5mg/mL graphene oxide dispersion liquid by deionized water, adding 5mLHBr aqueous solution (the mass percentage of HBr is 47%), reacting for 12 hours at the stirring speed of 1000r/min and the room temperature environment, adding oxalic acid, and continuing to react for 4 hours at the stirring speed of 1000r/min and the room temperature environment, wherein the mass ratio of graphene oxide, HBr aqueous solution and oxalic acid is 0.075:7.45:1.5, centrifuging for 5min at a rotating speed of 10000r/min after the reaction, taking a precipitate, washing the precipitate with deionized water for 3 times, and drying for 4h at a temperature of 40 ℃ to obtain carboxylated graphene oxide; the mass ratio is 30: mixing 6000 carboxylated graphene oxide and thionyl chloride, performing ultrasonic dispersion at a frequency of 30kHz for 40min, reacting at 70 ℃ for 32h, and performing reduced pressure distillation at 0.08MPa after the reaction to obtain acyl chloride graphene oxide;
step (2) adding acyl chloride graphene oxide into ethyl acetate, and dropwise adding an ethyl acetate solution of tri-n-butyl tin hydride at the temperature of 0 ℃ in a nitrogen atmosphere, wherein the mass ratio of the acyl chloride graphene oxide to the ethyl acetate solution of the ethyl acetate to the tri-n-butyl tin hydride is 25:400:285, the ethyl acetate solution of the tri-n-butyltin hydride is prepared from the tri-n-butyltin hydride and ethyl acetate according to a mass ratio of 45:240, stirring for 30min at the temperature of 0 ℃, heating to room temperature, maintaining the room temperature for 14h, filtering after the reaction, and drying for 2h at the temperature of 90 ℃ to obtain the aldehyde graphene oxide;
step (3) adding chitosan and aldehyde graphene oxide into ethanol, adding glacial acetic acid, and reacting for 4 hours at the temperature of 70 ℃, wherein the mass ratio of the aldehyde graphene oxide to the ethanol to the chitosan to the glacial acetic acid is 150:1900:300:90, filtering, washing and drying for 2 hours at the temperature of 90 ℃ after the reaction to obtain modified graphene oxide;
step (4) adding hexagonal boron nitride into 5mol/L sodium hydroxide aqueous solution, wherein the mass ratio of the hexagonal boron nitride to the sodium hydroxide aqueous solution is 1:60, performing ultrasonic dispersion for 50min at the frequency of 30kHz, stirring for 12h at the temperature of 70 ℃ at the stirring speed of 2200r/min, cooling to room temperature, performing suction filtration, washing filter residues with deionized water until the filter residues are neutral, and drying for 30h at the temperature of 70 ℃ to obtain hydroxylated hexagonal boron nitride; ethanol, hydroxylated hexagonal boron nitride and epoxypropyl trimethoxysilane are mixed according to the mass ratio of 4250:100:50, reacting for 10 hours at 110 ℃, filtering after the reaction, washing filter residues by using ethanol, and drying for 10 hours at 90 ℃ to obtain epoxy modified hexagonal boron nitride;
step (5) epoxy modified hexagonal boron nitride, modified graphene oxide, tetrahydrofuran and N-methyldiethanolamine according to the mass ratio of 90:70:4000:16, mixing, reacting for 6 hours at 110 ℃, filtering, washing, and drying for 7 hours at 70 ℃ to obtain cool and antibacterial functional powder;
step (6) the mass ratio is 7:90, mixing the cool antibacterial functional powder with nylon 6 master batch, melt spinning at 235 ℃, and chopping to obtain modified nylon fibers;
step (7) modified nylon fiber, cotton fiber and bamboo fiber according to the mass ratio of 3:1:1, and then knitting and weaving the inner layer yarns by using a weft knitting circular knitting machine to obtain the inner layer fabric, wherein the English count of the inner layer yarns is 45s, and the gram weight of the inner layer fabric is 250g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the Polyester fiber, bamboo fiber and apocynum fiber according to the mass ratio of 5:1:1, and then knitting and weaving the outer layer yarns by using a knitting weft knitting circular knitting machine to obtain an outer layer fabric, wherein the English count of the outer layer yarns is 45s, and the gram weight of the outer layer fabric is 250g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the And after the inner layer fabric and the outer layer fabric are aligned and laminated, sewing the shaped inner layer fabric and the shaped outer layer fabric by using a pure cotton sewing thread with the English count of 40s through a multi-layer fabric quilting machine to obtain the cool antibacterial fabric containing the inorganic composite nylon.
Example 4
Preparing graphene oxide into 2.5mg/mL graphene oxide dispersion liquid by deionized water, adding 5mLHBr aqueous solution (the mass percentage of HBr is 47%), reacting for 12 hours at the stirring speed of 1000r/min and the room temperature environment, adding oxalic acid, and continuing to react for 4 hours at the stirring speed of 1000r/min and the room temperature environment, wherein the mass ratio of graphene oxide, HBr aqueous solution and oxalic acid is 0.075:7.45:1.5, centrifuging for 5min at a rotating speed of 10000r/min after the reaction, taking a precipitate, washing the precipitate with deionized water for 3 times, and drying for 4h at a temperature of 40 ℃ to obtain carboxylated graphene oxide; the mass ratio is 35:7000 and thionyl chloride are mixed, ultrasonic dispersion is carried out for 35min at the frequency of 35kHz, reaction is carried out for 28h at the temperature of 73 ℃, and after the reaction, decompression distillation is carried out at the pressure of 0.08MPa, thus obtaining the acyl chloride graphene oxide;
step (2) adding acyl chloride graphene oxide into ethyl acetate, and dropwise adding an ethyl acetate solution of tri-n-butyl tin hydride at the temperature of 0 ℃ in a nitrogen atmosphere, wherein the mass ratio of the acyl chloride graphene oxide to the ethyl acetate solution of the ethyl acetate to the tri-n-butyl tin hydride is 27.5:500:300, the ethyl acetate solution of the tri-n-butyl tin hydride is prepared from the tri-n-butyl tin hydride and ethyl acetate according to a mass ratio of 55:245, stirring for 30min at the temperature of 0 ℃, heating to room temperature, keeping the room temperature for reaction for 13.5h, filtering after the reaction, and drying for 1.5h at the temperature of 95 ℃ to obtain the aldehyde graphene oxide;
step (3) adding chitosan and aldehyde graphene oxide into ethanol, adding glacial acetic acid, and reacting for 3 hours at the temperature of 75 ℃, wherein the mass ratio of the aldehyde graphene oxide to the ethanol to the chitosan to the glacial acetic acid is 175:2150:350:95, after the reaction, filtering, washing and drying for 1.5 hours at the temperature of 95 ℃ to obtain modified graphene oxide;
step (4) adding hexagonal boron nitride into 5mol/L sodium hydroxide aqueous solution, wherein the mass ratio of the hexagonal boron nitride to the sodium hydroxide aqueous solution is 1:65, performing ultrasonic dispersion for 45min at the frequency of 35kHz, stirring for 11h at the temperature of 75 ℃ at the stirring speed of 2500r/min, cooling to room temperature, performing suction filtration, washing filter residues with deionized water until the filter residues are neutral, and drying at the temperature of 75 ℃ for 27h to obtain hydroxylated hexagonal boron nitride; ethanol, hydroxylated hexagonal boron nitride and epoxypropyl trimethoxysilane are mixed according to the mass ratio of 4875:100:55, reacting for 9 hours at 115 ℃, filtering after the reaction, washing filter residues by using ethanol, and drying for 9 hours at 95 ℃ to obtain epoxy modified hexagonal boron nitride;
step (5) epoxy modified hexagonal boron nitride, modified graphene oxide, tetrahydrofuran and N-methyldiethanolamine according to a mass ratio of 95:75:4500:19, reacting for 5 hours at 115 ℃, filtering, washing, and drying for 6.5 hours at 75 ℃ to obtain cool antibacterial functional powder;
step (6) the mass ratio is 8:95, mixing the cool antibacterial functional powder with nylon 6 master batch, melt spinning at 240 ℃, and chopping to obtain modified nylon fibers;
step (7) modified nylon fiber, cotton fiber and bamboo fiber according to the mass ratio of 4:1:1, and then knitting and weaving the inner layer yarns by using a weft knitting circular knitting machine to obtain the inner layer fabric, wherein the English count of the inner layer yarns is 55s, and the gram weight of the inner layer fabric is 260g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the Polyester fiber, bamboo fiber and apocynum fiber according to the mass ratio of 7:1:1 blending to obtain outer layer yarn, and then knitting weft knitting circular knitting machineKnitting and weaving the outer layer yarns to obtain an outer layer fabric, wherein the English count of the outer layer yarns is 55s, and the gram weight of the outer layer fabric is 260g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the And after the inner layer fabric and the outer layer fabric are aligned and laminated, sewing the shaped inner layer fabric and the shaped outer layer fabric by using a pure cotton sewing thread with the English count of 40s through a multi-layer fabric quilting machine to obtain the cool antibacterial fabric containing the inorganic composite nylon.
Example 5
Preparing graphene oxide into 2.5mg/mL graphene oxide dispersion liquid by deionized water, adding 5mLHBr aqueous solution (the mass percentage of HBr is 47%), reacting for 12 hours at the stirring speed of 1000r/min and the room temperature environment, adding oxalic acid, and continuing to react for 4 hours at the stirring speed of 1000r/min and the room temperature environment, wherein the mass ratio of graphene oxide, HBr aqueous solution and oxalic acid is 0.075:7.45:1.5, centrifuging for 5min at a rotating speed of 10000r/min after the reaction, taking a precipitate, washing the precipitate with deionized water for 3 times, and drying for 4h at a temperature of 40 ℃ to obtain carboxylated graphene oxide; the mass ratio is 40:8000 carboxylated graphene oxide and thionyl chloride are mixed, dispersed for 30min under the frequency of 40kHz, reacted for 24h at the temperature of 75 ℃, and distilled under reduced pressure under the pressure of 0.08MPa after the reaction, so as to obtain the acyl chloride graphene oxide;
step (2) adding acyl chloride graphene oxide into ethyl acetate, and dropwise adding an ethyl acetate solution of tri-n-butyl tin hydride at the temperature of 0 ℃ in a nitrogen atmosphere, wherein the mass ratio of the acyl chloride graphene oxide to the ethyl acetate solution of the ethyl acetate to the tri-n-butyl tin hydride is 30:600:310, the ethyl acetate solution of tri-n-butyltin hydride is prepared from tri-n-butyltin hydride and ethyl acetate according to a mass ratio of 60:250, stirring for 30min at the temperature of 0 ℃, heating to room temperature, maintaining the room temperature for 13h, filtering after the reaction, and drying for 1h at the temperature of 100 ℃ to obtain the aldehyde graphene oxide;
step (3) adding chitosan and aldehyde graphene oxide into ethanol, adding glacial acetic acid, and reacting for 2 hours at the temperature of 80 ℃, wherein the mass ratio of the aldehyde graphene oxide to the ethanol to the chitosan to the glacial acetic acid is 200:2400:400:100, after the reaction, filtering, washing and drying for 1h at the temperature of 100 ℃ to obtain modified graphene oxide;
step (4) adding hexagonal boron nitride into 5mol/L sodium hydroxide aqueous solution, wherein the mass ratio of the hexagonal boron nitride to the sodium hydroxide aqueous solution is 1:70, performing ultrasonic dispersion for 40min at a frequency of 40kHz, stirring for 10h at a stirring speed of 2800r/min and a temperature of 80 ℃, cooling to room temperature, performing suction filtration, washing filter residues with deionized water until the filter residues are neutral, and drying at 80 ℃ for 24h to obtain hydroxylated hexagonal boron nitride; ethanol, hydroxylated hexagonal boron nitride and epoxypropyl trimethoxysilane are mixed according to the mass ratio of 5500:100:60, reacting for 8 hours at 120 ℃, filtering after the reaction, washing filter residues by using ethanol, and drying for 8 hours at 100 ℃ to obtain epoxy modified hexagonal boron nitride;
step (5) epoxy modified hexagonal boron nitride, modified graphene oxide, tetrahydrofuran and N-methyldiethanolamine according to the mass ratio of 100:80:5000:22, mixing, reacting for 4 hours at 120 ℃, filtering, washing, and drying for 6 hours at 80 ℃ to obtain cool antibacterial functional powder;
step (6) the mass ratio is 9:100, mixing the cool antibacterial functional powder with nylon 6 master batch, melt spinning at 240 ℃, and chopping to obtain modified nylon fibers;
step (7) modified nylon fiber, cotton fiber and bamboo fiber according to the mass ratio of 5:1:1, and then knitting and weaving the inner layer yarns by using a weft knitting circular knitting machine to obtain the inner layer fabric, wherein the English count of the inner layer yarns is 55s, and the gram weight of the inner layer fabric is 260g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the Polyester fiber, bamboo fiber and apocynum fiber according to the mass ratio of 9:1:1, and then knitting and weaving the outer layer yarns by using a knitting weft knitting circular knitting machine to obtain an outer layer fabric, wherein the English count of the outer layer yarns is 55s, and the gram weight of the outer layer fabric is 260g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the And after the inner layer fabric and the outer layer fabric are aligned and laminated, sewing the shaped inner layer fabric and the shaped outer layer fabric by using a pure cotton sewing thread with the English count of 40s through a multi-layer fabric quilting machine to obtain the cool antibacterial fabric containing the inorganic composite nylon.
Comparative example 1
Preparing graphene oxide into 2.5mg/mL graphene oxide dispersion liquid by deionized water, adding 5mLHBr aqueous solution (the mass percentage of HBr is 47%), reacting for 12 hours at the stirring speed of 1000r/min and the room temperature environment, adding oxalic acid, and continuing to react for 4 hours at the stirring speed of 1000r/min and the room temperature environment, wherein the mass ratio of graphene oxide, HBr aqueous solution and oxalic acid is 0.075:7.45:1.5, centrifuging for 5min at a rotating speed of 10000r/min after the reaction, taking a precipitate, washing the precipitate with deionized water for 3 times, and drying for 4h at a temperature of 40 ℃ to obtain carboxylated graphene oxide; the mass ratio is 20: mixing 4000 carboxylated graphene oxide and thionyl chloride, performing ultrasonic dispersion at a frequency of 20kHz for 50min, reacting at 65 ℃ for 40h, and performing reduced pressure distillation at 0.08MPa after the reaction to obtain acyl chloride graphene oxide;
step (2) adding acyl chloride graphene oxide into ethyl acetate, and dropwise adding an ethyl acetate solution of tri-n-butyl tin hydride at the temperature of 0 ℃ in a nitrogen atmosphere, wherein the mass ratio of the acyl chloride graphene oxide to the ethyl acetate solution of the ethyl acetate to the tri-n-butyl tin hydride is 20:200:270, the ethyl acetate solution of the tri-n-butyl tin hydride is prepared from the tri-n-butyl tin hydride and ethyl acetate according to the mass ratio of 40:230, stirring for 30min at the temperature of 0 ℃, heating to room temperature, maintaining the room temperature for reaction for 15h, filtering after the reaction, and drying for 3h at the temperature of 80 ℃ to obtain the aldehyde graphene oxide;
step (3) adding chitosan and aldehyde graphene oxide into ethanol, adding glacial acetic acid, and reacting for 6 hours at the temperature of 60 ℃, wherein the mass ratio of the aldehyde graphene oxide to the ethanol to the chitosan to the glacial acetic acid is 100:1400:200:80, after the reaction, filtering, washing and drying for 3 hours at the temperature of 80 ℃ to obtain modified graphene oxide;
step (4) adding hexagonal boron nitride into 5mol/L sodium hydroxide aqueous solution, wherein the mass ratio of the hexagonal boron nitride to the sodium hydroxide aqueous solution is 1:50, performing ultrasonic dispersion for 60min at the frequency of 20kHz, stirring for 14h at the temperature of 60 ℃ at the stirring speed of 1600r/min, cooling to room temperature, performing suction filtration, washing filter residues with deionized water until the filter residues are neutral, and drying at 60 ℃ for 36h to obtain hydroxylated hexagonal boron nitride; ethanol, hydroxylated hexagonal boron nitride and epoxypropyl trimethoxy silane are mixed according to the mass ratio of 3000:100:40, reacting for 12 hours at 100 ℃, filtering after the reaction, washing filter residues by using ethanol, and drying for 12 hours at 80 ℃ to obtain epoxy modified hexagonal boron nitride;
step (5) epoxy modified hexagonal boron nitride and modified graphene oxide are mixed according to the mass ratio of 80:60, mixing to obtain cool antibacterial functional powder;
step (6) the mass ratio is 5:80 and nylon 6 master batch are mixed, melt-spun at 230 ℃ and chopped to obtain modified nylon fibers;
step (7) modified nylon fiber, cotton fiber and bamboo fiber according to the mass ratio of 1:1:1, and then knitting and weaving the inner layer yarns by using a weft knitting circular knitting machine to obtain the inner layer fabric, wherein the English count of the inner layer yarns is 45s, and the gram weight of the inner layer fabric is 250g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the Polyester fiber, bamboo fiber and apocynum fiber according to the mass ratio of 1:1:1, and then knitting and weaving the outer layer yarns by using a knitting weft knitting circular knitting machine to obtain an outer layer fabric, wherein the English count of the outer layer yarns is 45s, and the gram weight of the outer layer fabric is 250g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the And after the inner layer fabric and the outer layer fabric are aligned and laminated, sewing the shaped inner layer fabric and the shaped outer layer fabric by using a pure cotton sewing thread with the English count of 40s through a multi-layer fabric quilting machine to obtain the cool antibacterial fabric containing the inorganic composite nylon.
Comparative example 2
Preparing graphene oxide into 2.5mg/mL graphene oxide dispersion liquid by deionized water, adding 5mLHBr aqueous solution (the mass percentage of HBr is 47%), reacting for 12 hours at the stirring speed of 1000r/min and the room temperature environment, adding oxalic acid, and continuing to react for 4 hours at the stirring speed of 1000r/min and the room temperature environment, wherein the mass ratio of graphene oxide, HBr aqueous solution and oxalic acid is 0.075:7.45:1.5, centrifuging for 5min at a rotating speed of 10000r/min after the reaction, taking a precipitate, washing the precipitate with deionized water for 3 times, and drying for 4h at a temperature of 40 ℃ to obtain carboxylated graphene oxide; the mass ratio is 20: mixing 4000 carboxylated graphene oxide and thionyl chloride, performing ultrasonic dispersion at a frequency of 20kHz for 50min, reacting at 65 ℃ for 40h, and performing reduced pressure distillation at 0.08MPa after the reaction to obtain acyl chloride graphene oxide;
step (2) adding acyl chloride graphene oxide into ethyl acetate, and dropwise adding an ethyl acetate solution of tri-n-butyl tin hydride at the temperature of 0 ℃ in a nitrogen atmosphere, wherein the mass ratio of the acyl chloride graphene oxide to the ethyl acetate solution of the ethyl acetate to the tri-n-butyl tin hydride is 20:200:270, the ethyl acetate solution of the tri-n-butyl tin hydride is prepared from the tri-n-butyl tin hydride and ethyl acetate according to the mass ratio of 40:230, stirring for 30min at the temperature of 0 ℃, heating to room temperature, maintaining the room temperature for reaction for 15h, filtering after the reaction, and drying for 3h at the temperature of 80 ℃ to obtain the aldehyde graphene oxide;
step (3) adding chitosan and aldehyde graphene oxide into ethanol, adding glacial acetic acid, and reacting for 6 hours at the temperature of 60 ℃, wherein the mass ratio of the aldehyde graphene oxide to the ethanol to the chitosan to the glacial acetic acid is 100:1400:200:80, after the reaction, filtering, washing and drying for 3 hours at the temperature of 80 ℃ to obtain modified graphene oxide;
and (4) mixing the materials with the mass ratio of 5:80, mixing modified graphene oxide with nylon 6 master batch, melt spinning at 230 ℃, and chopping to obtain graphene oxide modified nylon fiber;
step (5) graphene oxide modified nylon fiber, cotton fiber and bamboo fiber according to the mass ratio of 1:1:1, and then knitting and weaving the inner layer yarns by using a weft knitting circular knitting machine to obtain the inner layer fabric, wherein the English count of the inner layer yarns is 45s, and the gram weight of the inner layer fabric is 250g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the Polyester fiber, bamboo fiber and apocynum fiber according to the mass ratio of 1:1:1, and then knitting and weaving the outer layer yarns by using a knitting weft knitting circular knitting machine to obtain an outer layer fabric, wherein the English count of the outer layer yarns is 45s, and the gram weight of the outer layer fabric is 250g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the And after the inner layer fabric and the outer layer fabric are aligned and laminated, sewing the shaped inner layer fabric and the shaped outer layer fabric by using a pure cotton sewing thread with the English count of 40s through a multi-layer fabric quilting machine to obtain the cool antibacterial fabric containing the inorganic composite nylon.
In each example and comparative example of the present invention, graphene oxide was purchased from Xuancheng Jinrui New Material Co., ltd, model number was JR05, and average particle diameter was 5nm; the chitosan supplier is preferably Shandong Okang Biotechnology Co., ltd; tetrahydrofuran suppliers preferably, tianjin Miou reagent Co., ltd, are analytically pure; nylon 6 master batch was purchased from Shanghai pine chemical industry limited; hexagonal boron nitride was purchased from Zhejiang submicron technologies limited; other reagents used in the present invention are all commercially available.
The cool antibacterial fabrics containing the inorganic composite nylon prepared in examples 1-5 and comparative examples 1-2 were selected and respectively marked as samples 1-7, and were subjected to corresponding tests.
(1) Cooling test: the fabrics were tested for cooling performance according to GB/T35263-2017 detection and evaluation of textile contact instant cooling performance, and the test results are shown in Table 1.
According to the test results shown in table 1, both graphene oxide and hexagonal boron nitride are of a layered honeycomb structure, and are excellent heat conduction materials, and especially the heat conduction performance of hexagonal boron nitride is superior to that of most metal materials. After ultrasonic stripping and modification, the hexagonal boron nitride improves the dispersibility and the interface effect with the polymer, and a continuous heat conducting particle passage is formed by mutually overlapping the inside of the matrix and the graphene oxide, and heat is mainly transferred along a heat conducting network. After the graphene oxide is modified, the dispersibility is obviously improved, and the graphene oxide is connected with the hexagonal boron nitride through chemical bonds, so that the graphene oxide is more durable in comparison with the blending connection mode of the graphene oxide and the hexagonal boron nitride, and the heat conducting property of the graphene oxide is more durable. In comparative example 1, the modified graphene oxide and the epoxy modified hexagonal boron nitride are compounded, and are not connected through chemical bonds, so that the heat conduction performance of the modified graphene oxide is lower than that of example 1, and the instant sensing value is reduced; the hexagonal boron nitride in the comparative example 2 has a stable structure, the hydroxyl utilization rate of the surface is low under the condition of no ultrasonic treatment, and the dispersibility and the interface compatibility are lower than those of the epoxy modified hexagonal boron nitride, so that the heat conduction performance in the comparative example 2 is poorer than that in the comparative example 1;
(2) Antibacterial performance test: evaluation of antibacterial Properties of textiles with test Standard GB/T20944.3-2008 part 3: the antibacterial skin-friendly webbing of examples 1-5 and comparative examples 1-2 were subjected to antibacterial performance test by oscillation method, and experimental strains were selected from E.coli and Staphylococcus aureus, and the test results are shown in Table 2.
From the test results of table 2, it can be seen that both graphene oxide and chitosan have excellent bacteriostatic ability. The chitosan has good biocompatibility and antibacterial property, and the aldehyde graphene oxide and the chitosan are combined to generate Schiff base, so that the antibacterial effect is further improved; the modified graphene oxide and the epoxy modified hexagonal boron nitride are combined to generate Schiff base, so that the organic and inorganic antibacterial effects are further improved. In comparative example 1, the lack of the condition for producing schiff base reduced the bacteriostatic effect compared with example 1; in comparative example 2, hexagonal boron nitride was used as a heat conductive material, and the dispersibility in the matrix was incomplete, which was not conducive to bacteriostasis, and the bacteriostatic effect was lower than that of comparative example 1.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The preparation method of the cool antibacterial fabric containing the inorganic composite nylon is characterized by comprising the following steps of:
preparing graphene oxide into graphene oxide dispersion liquid by deionized water, adding HBr aqueous solution, reacting, adding oxalic acid, continuing the reaction, centrifuging, washing and drying to obtain carboxylated graphene oxide; mixing carboxylated graphene oxide and thionyl chloride, performing ultrasonic dispersion, reacting, and performing reduced pressure distillation to obtain acyl chloride graphene oxide;
step (2) adding acyl chloride graphene oxide into ethyl acetate, dropwise adding ethyl acetate solution of tri-n-butyl tin hydride, stirring, reacting, filtering after the reaction, and drying to obtain aldehyde graphene oxide;
step (3) adding chitosan and aldehyde graphene oxide into ethanol, adding glacial acetic acid, reacting, filtering, washing and drying to obtain modified graphene oxide;
step (4) mixing epoxy modified hexagonal boron nitride, modified graphene oxide, tetrahydrofuran and N-methyldiethanolamine, reacting, filtering, washing and drying to obtain cool antibacterial functional powder;
step (5) mixing the cool antibacterial functional powder with nylon master batch, and spinning to obtain modified nylon fiber;
step (6), spinning the inner layer raw material to obtain an inner layer fabric; weaving the outer layer raw materials to obtain an outer layer fabric; after the inner layer fabric and the outer layer fabric are aligned and overlapped, stitching to obtain the cool antibacterial fabric containing the inorganic composite nylon; wherein the inner layer raw material comprises modified nylon fiber, cotton fiber and bamboo fiber; the outer layer raw materials comprise polyester fiber, bamboo fiber and apocynum fiber.
2. The method for preparing the cool antibacterial fabric containing the inorganic composite nylon according to claim 1, wherein in the step (1): when preparing carboxylated graphene oxide, the mass ratio of graphene oxide, HBr aqueous solution and oxalic acid is 0.075:7.45:1.5, the reaction condition is stirring and reacting for 12 hours at room temperature, and the continuous reaction condition is stirring and reacting for 4 hours at room temperature; when preparing the acyl chloride graphene oxide, the mass ratio of carboxylated graphene oxide to thionyl chloride is (20-40): (4000-8000) under the reaction condition of 65-75 ℃ for 24-40h.
3. The method for preparing the cool antibacterial fabric containing the inorganic composite chinlon according to claim 1, wherein in the step (2), the mass ratio of the ethyl acetate solution of the acyl chloride graphene oxide, the ethyl acetate and the tri-n-butyl tin hydride is (20-30): (200-600): (270-310), the dripping condition of the ethyl acetate solution of the tri-n-butyl tin hydride is that the reaction is carried out for 13-15h at room temperature in 0 ℃ and inert gas atmosphere.
4. The method for preparing the cool antibacterial fabric containing the inorganic composite nylon according to claim 1, wherein in the step (3), the reaction condition is that the reaction is carried out for 2-6 hours at the temperature of 60-80 ℃.
5. The method for preparing the cool antibacterial fabric containing the inorganic composite chinlon according to claim 1, wherein in the step (4), the mass ratio of epoxy modified hexagonal boron nitride to modified graphene oxide to tetrahydrofuran to N-methyldiethanolamine is (80-100): (60-80): (3000-5000): (10-22).
6. The method for preparing the cool antibacterial fabric containing the inorganic composite nylon, which is disclosed in claim 1, is characterized in that the epoxy modified hexagonal boron nitride in the step (4) is prepared by the following steps:
adding hexagonal boron nitride into a sodium hydroxide aqueous solution, performing ultrasonic dispersion, stirring for reaction, cooling, performing suction filtration, washing and drying to obtain hydroxylated hexagonal boron nitride; mixing ethanol, hydroxylated hexagonal boron nitride and epoxypropyl trimethoxy silane, reacting, filtering, washing and drying to obtain the epoxy modified hexagonal boron nitride.
7. The method for preparing the cool antibacterial fabric containing inorganic composite nylon according to claim 1, wherein the spinning in the step (5) comprises melt spinning and chopping after the melt spinning.
8. The method for preparing the cool antibacterial fabric containing the inorganic composite nylon, which is disclosed in claim 1, is characterized in that in the step (6), modified nylon fiber, cotton fiber and bamboo fiber are blended to prepare inner layer yarns, and then knitting and weaving are carried out on the inner layer yarns by using a knitting weft knitting circular knitting machine to obtain the inner layer fabric; blending polyester fiber, bamboo fiber and apocynum fiber to obtain outer layer yarns, and knitting and weaving the outer layer yarns by using a weft knitting circular knitting machine to obtain outer layer fabrics; and (3) after the inner layer fabric and the outer layer fabric are aligned and overlapped, stitching to obtain the cool antibacterial fabric containing the inorganic composite nylon.
9. A cool antibacterial fabric containing inorganic composite nylon, prepared by the preparation method of the cool antibacterial fabric containing inorganic composite nylon according to any one of claims 1 to 8.
10. The use of the cool antibacterial fabric containing inorganic composite nylon as claimed in claim 9 in clothing.
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Effective date of registration: 20231024 Address after: Floor 4, Building A7, Standardization Plant, Economic Development Zone, Guoyang County, Bozhou City, Anhui Province, 236000 Applicant after: Woyang County Libaihui Clothing Co.,Ltd. Address before: 515000 Shantou Xingyutai Textile Co., Ltd., Xianbo Qiweiyang Industrial Zone, Gurao Town, Chaoyang District, Shantou City, Guangdong Province Applicant before: SHANTOU XINGYUTAI WEAVING Co.,Ltd. |