CN117587561A - High-elasticity nylon-spandex coated yarn, preparation method thereof and application thereof in fabric - Google Patents
High-elasticity nylon-spandex coated yarn, preparation method thereof and application thereof in fabric Download PDFInfo
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- CN117587561A CN117587561A CN202410068818.0A CN202410068818A CN117587561A CN 117587561 A CN117587561 A CN 117587561A CN 202410068818 A CN202410068818 A CN 202410068818A CN 117587561 A CN117587561 A CN 117587561A
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- Prior art keywords
- reaction
- modified
- silver
- nylon
- spandex
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- 229920002334 Spandex Polymers 0.000 title claims abstract description 92
- 239000004759 spandex Substances 0.000 title claims abstract description 92
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000004744 fabric Substances 0.000 title claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 105
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 90
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 79
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 79
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000004952 Polyamide Substances 0.000 claims abstract description 67
- 229920002647 polyamide Polymers 0.000 claims abstract description 67
- 238000002156 mixing Methods 0.000 claims abstract description 64
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000000654 additive Substances 0.000 claims abstract description 47
- 230000000996 additive effect Effects 0.000 claims abstract description 47
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052709 silver Inorganic materials 0.000 claims abstract description 42
- 239000004332 silver Substances 0.000 claims abstract description 42
- 239000004677 Nylon Substances 0.000 claims abstract description 41
- 229920001778 nylon Polymers 0.000 claims abstract description 41
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000007864 aqueous solution Substances 0.000 claims abstract description 38
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims abstract description 38
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 150000003378 silver Chemical class 0.000 claims abstract description 32
- -1 alkyl quaternary ammonium salt modified montmorillonite Chemical class 0.000 claims abstract description 27
- 229920002413 Polyhexanide Polymers 0.000 claims abstract description 25
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 20
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 claims abstract description 19
- NQTADLQHYWFPDB-UHFFFAOYSA-N N-Hydroxysuccinimide Chemical compound ON1C(=O)CCC1=O NQTADLQHYWFPDB-UHFFFAOYSA-N 0.000 claims abstract description 19
- LMDZBCPBFSXMTL-UHFFFAOYSA-N 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide Substances CCN=C=NCCCN(C)C LMDZBCPBFSXMTL-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000001361 adipic acid Substances 0.000 claims abstract description 18
- 235000011037 adipic acid Nutrition 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 229920001971 elastomer Polymers 0.000 claims abstract description 12
- 239000000806 elastomer Substances 0.000 claims abstract description 12
- 125000004368 propenyl group Chemical group C(=CC)* 0.000 claims abstract description 7
- 238000002074 melt spinning Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 38
- 238000001035 drying Methods 0.000 claims description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 27
- 238000001914 filtration Methods 0.000 claims description 24
- 239000008055 phosphate buffer solution Substances 0.000 claims description 24
- 239000007795 chemical reaction product Substances 0.000 claims description 20
- 238000000576 coating method Methods 0.000 claims description 20
- 238000009987 spinning Methods 0.000 claims description 20
- 239000011248 coating agent Substances 0.000 claims description 19
- 239000012043 crude product Substances 0.000 claims description 18
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 16
- GCNNVAWVYJUFCO-UHFFFAOYSA-N ethanol;hexanedioic acid Chemical compound CCO.OC(=O)CCCCC(O)=O GCNNVAWVYJUFCO-UHFFFAOYSA-N 0.000 claims description 15
- 239000002244 precipitate Substances 0.000 claims description 14
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 13
- 229920000570 polyether Polymers 0.000 claims description 13
- 238000005245 sintering Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 230000020477 pH reduction Effects 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 239000004753 textile Substances 0.000 abstract description 4
- 230000000379 polymerizing effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 19
- 238000005253 cladding Methods 0.000 description 15
- 230000008569 process Effects 0.000 description 11
- 238000012360 testing method Methods 0.000 description 7
- 230000003115 biocidal effect Effects 0.000 description 6
- 230000001877 deodorizing effect Effects 0.000 description 6
- 238000009210 therapy by ultrasound Methods 0.000 description 6
- 229920000800 acrylic rubber Polymers 0.000 description 5
- 150000001412 amines Chemical class 0.000 description 5
- 229920000058 polyacrylate Polymers 0.000 description 5
- 230000000630 rising effect Effects 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000003242 anti bacterial agent Substances 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 4
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000006068 polycondensation reaction Methods 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 238000007112 amidation reaction Methods 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010954 inorganic particle Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000008363 phosphate buffer Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- AKGZDINYLOSBTE-UHFFFAOYSA-N [(e)-n'-(diaminomethylideneamino)carbamimidoyl]azanium;chloride Chemical compound Cl.NC(=N)NN=C(N)N AKGZDINYLOSBTE-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- SLLGSVYJOJWVMY-UHFFFAOYSA-N magnesium silver oxygen(2-) Chemical compound [O-2].[Mg+2].[Ag+] SLLGSVYJOJWVMY-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007378 ring spinning Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Classifications
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/22—Yarns or threads characterised by constructional features, e.g. blending, filament/fibre
- D02G3/32—Elastic yarns or threads ; Production of plied or cored yarns, one of which is elastic
- D02G3/328—Elastic yarns or threads ; Production of plied or cored yarns, one of which is elastic containing elastane
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
- D02G3/04—Blended or other yarns or threads containing components made from different materials
- D02G3/045—Blended or other yarns or threads containing components made from different materials all components being made from artificial or synthetic material
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/22—Yarns or threads characterised by constructional features, e.g. blending, filament/fibre
- D02G3/38—Threads in which fibres, filaments, or yarns are wound with other yarns or filaments, e.g. wrap yarns, i.e. strands of filaments or staple fibres are wrapped by a helically wound binder yarn
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/44—Yarns or threads characterised by the purpose for which they are designed
- D02G3/441—Yarns or threads with antistatic, conductive or radiation-shielding properties
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/44—Yarns or threads characterised by the purpose for which they are designed
- D02G3/449—Yarns or threads with antibacterial properties
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/02—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyamides
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/10—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyurethanes
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/06—Load-responsive characteristics
- D10B2401/061—Load-responsive characteristics elastic
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/16—Physical properties antistatic; conductive
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to the technical field of textile, and discloses a high-elasticity nylon-spandex coated yarn, a preparation method thereof and application thereof in fabric. The method comprises the following steps: mixing silver nitrate aqueous solution, magnesium nitrate aqueous solution and citric acid for reaction to obtain silver-loaded magnesium oxide; acidifying silver-carrying magnesia to obtain modified silver-carrying magnesia; reacting modified silver-loaded magnesium oxide, 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, N-hydroxysuccinimide and polyhexamethylene biguanide hydrochloride to obtain an antibacterial additive; polymerizing polyetheramine, adipic acid and an antibacterial additive to obtain modified polyamide; mixing the propenyl elastomer, the alkyl quaternary ammonium salt modified montmorillonite, the modified polyamide and the polyamide, and carrying out melt spinning to obtain modified nylon filaments; the high-elasticity nylon-spandex coated yarn formed by the modified nylon filaments and the spandex filaments has wide application prospects in fabrics.
Description
Technical Field
The invention relates to the technical field of textile, in particular to a high-elasticity nylon-spandex coated yarn, a preparation method thereof and application thereof in fabric.
Background
The cladding yarn is formed by compounding two or more fibers, and can make up the defects of single-component fibers in performance and play the advantages of the composite fibers. The covered yarn has extremely wide application as a large branch of composite spinning.
The covered yarn is generally composed of an inner core yarn and an outer covered yarn covering the core yarn, and spandex is a fiber having high elasticity, and only a small amount of spandex is required to give excellent elasticity to yarns, fabrics, and the like. In the preparation of the covered yarn, spandex is often used as the core yarn to impart excellent elasticity to the covered yarn. The current common coating yarn is nylon-spandex coating yarn, nylon can be used as an outer coating yarn to well protect core yarn spandex, but the mechanical property, elasticity and antistatic ability of the nylon serving as the outer coating yarn are poor, the elasticity of the coating yarn after coating the spandex is reduced, and the common nylon-spandex coating yarn has no antibacterial property, so that the application of the coating yarn in fabric is limited.
The prior art, such as Chinese patent application CN106192119A, discloses an antibacterial nylon covered yarn and a manufacturing method thereof, wherein the antibacterial nylon covered yarn is prepared by taking spandex filaments as outer covered yarns and antibacterial modified nylon filaments as core yarns after covering. The obtained antibacterial nylon cladding yarn has permanent antibacterial effect. However, the prepared coated yarn takes spandex filaments as a coating layer, and because the mechanical property and the wear resistance of spandex are poor, more spandex filaments are exposed on the outer layer of the yarn body, and the spandex filaments are easy to be damaged by friction in the processing process and the using process, so that fatigue fracture and other conditions occur, and the coated yarn has no antistatic property, so that the application of the coated yarn in fabric is limited.
The prior art, such as chinese patent application CN113737344a, discloses an antibacterial deodorizing spandex covered yarn, which performs antibacterial deodorizing treatment on spandex filaments by adopting a two-soaking two-rolling finishing process, so that the spandex filaments are antibacterial and deodorizing, and meanwhile, the problems of uneven color light, poor yellowing aging quality and the like of the spandex filaments are avoided. The antibacterial deodorizing spandex filament added with the antibacterial agent is used as an outer cladding yarn to be combined with the core yarn spandex filament, and the prepared antibacterial deodorizing spandex cladding yarn has good antibacterial effect and deodorizing capability. But the nylon used as the outer cladding yarn in the prepared cladding yarn has poor mechanical property, elasticity and antistatic ability, the elasticity of the cladding yarn after the spandex is coated is reduced, and the application of the cladding yarn in fabric is limited.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the high-elasticity nylon-spandex coated yarn, the preparation method and the application thereof in the fabric.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the high-elasticity nylon-spandex coated yarn comprises the following steps:
step (1), mixing silver nitrate aqueous solution, magnesium nitrate aqueous solution and citric acid, reacting, drying after the reaction is finished, and sintering to obtain silver-loaded magnesium oxide; mixing silver-loaded magnesia, hydrochloric acid aqueous solution and water, carrying out acidification reaction, filtering, washing and drying after the reaction is finished to obtain modified silver-loaded magnesia;
step (2), mixing the modified silver-loaded magnesium oxide with a phosphate buffer solution, performing ultrasound, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, reacting, filtering after the reaction is finished, and washing to obtain a reaction product; mixing the reaction product with a phosphate buffer solution, adding a polyhexamethylene biguanide hydrochloride aqueous solution, continuing to react, centrifuging after the reaction is finished, taking a centrifugal precipitate, washing, and drying to obtain an antibacterial additive;
step (3), dropwise adding polyether amine-ethanol solution into adipic acid-ethanol solution, adding an antibacterial additive after dropwise adding, carrying out a first reaction, filtering after the reaction is finished, and drying to obtain a modified polyamide crude product; mixing the modified polyamide crude product with water, carrying out a second reaction, continuing the reaction after the reaction is finished, and cooling after the reaction is finished to obtain modified polyamide;
step (4), mixing the propenyl elastomer, the alkyl quaternary ammonium salt modified montmorillonite, the modified polyamide and the polyamide, and carrying out melt spinning to obtain modified nylon filaments; and coating the core yarn by using the spandex filaments as the core yarn and using modified nylon filaments to obtain the high-elasticity nylon-spandex coated yarn.
Preferably, in the step (1): the mass ratio of the silver nitrate to the magnesium nitrate to the citric acid is (0.1-1): 10: (8-10); the reaction conditions are as follows: stirring and reacting for 4-6h at 70-80 ℃; the drying conditions are as follows: drying at 130-150deg.C for 2-4 hr; the sintering conditions are as follows: heating to 600 ℃ and sintering for 2 hours, wherein the heating rate is 2-5 ℃/min.
Preferably, the aqueous silver nitrate solution comprises a 20wt% aqueous silver nitrate solution; the aqueous magnesium nitrate solution comprises 20wt% aqueous magnesium nitrate solution.
Preferably, in the step (1): the mass ratio of the silver-loaded magnesium oxide to the hydrochloric acid aqueous solution to the water is 1: (1.5-3): (10-20); the acidification reaction conditions are as follows: acidizing reaction at room temperature for 6-12h.
Preferably, the aqueous hydrochloric acid solution is a 1mol/L aqueous hydrochloric acid solution.
Preferably, in the step (2): the mass ratio of the modified silver-carrying magnesium oxide to the phosphate buffer solution is 1: (800-1000); the reaction conditions are as follows: reacting for 2 hours at room temperature at the rotating speed of 180-200 r/min; the mass ratio of the reaction product to the phosphate buffer solution is 1: (800-1000); the continuous reaction conditions are as follows: and continuing the reaction for 4-6h at the room temperature at the rotating speed of 180-200 r/min.
Preferably, in the step (2): the mass ratio of the modified silver-loaded magnesium oxide to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the N-hydroxysuccinimide to the polyhexamethylene biguanide hydrochloride is 1: (8-10): (8-10): (10-15).
Preferably, the polyhexamethylene biguanide hydrochloride aqueous solution comprises 20wt% polyhexamethylene biguanide hydrochloride aqueous solution.
Further, the pH value of the phosphate buffer solution mixed with the modified silver-loaded magnesium oxide is 5.5; the pH of the phosphate buffer solution mixed with the reaction product was 7.5.
Preferably, in the step (3): the mass ratio of polyetheramine, adipic acid and the antibacterial additive is 45:43: (1-5); the dropping conditions are as follows: dripping at room temperature for 20-30min; the first reaction conditions are as follows: the first reaction is carried out for 1 to 2 hours at the temperature of 40 to 50 ℃.
Preferably, in the step (3): the mass ratio of the modified polyamide crude product to water is 3:2; the second reaction conditions are as follows: reacting for 1-3h in nitrogen atmosphere at 90-110 ℃; the continuous reaction conditions are as follows: and continuing the reaction for 4-6h at the temperature of 250-260 ℃ in a nitrogen atmosphere.
Preferably, the polyetheramine-ethanol solution is prepared from polyetheramine and ethanol at room temperature in a mass ratio of (45-50): (250-320) mixing and dissolving to prepare the product; the adipic acid-ethanol solution is prepared from adipic acid and ethanol at 45 ℃ in a mass ratio of (43-50): (280-340) and is prepared by mixing and dissolving.
Further, the polyetheramine is polyetheramine EDR-148.
Preferably, in the step (4): the mass ratio of the propenyl elastomer to the alkyl quaternary ammonium salt modified montmorillonite to the modified polyamide to the polyamide is (5-10): (2-3): (10-20): (80-100); the melt spinning conditions are: melting at 220-260 deg.C, spinning at 1500-3200 m/min.
Preferably, in the step (4): the fineness of the modified nylon filament is 50-120D; the fineness of the spandex filament is 60-100D.
Preferably, the high-elasticity nylon-spandex coated yarn is prepared by adopting the preparation method of the high-elasticity nylon-spandex coated yarn.
Preferably, the application of the nylon-spandex coated yarn with high elasticity in the fabric is adopted.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, the silver is added to dope the magnesium oxide, and the obtained silver-loaded magnesium oxide has more excellent antibacterial capability. Meanwhile, as the magnesium oxide and the silver have conductivity, and the silver is doped in the magnesium oxide crystal, a network for transferring electrons is formed, and the leakage of charges is quickened, the nylon added with the silver-loaded magnesium oxide has antibacterial property and antistatic capability.
According to the invention, the surface of silver-loaded magnesium oxide is acidified, so that the carboxyl on the surface and the amino of polyhexamethylene biguanidine hydrochloride are subjected to amidation reaction, and the antibacterial additive is obtained. The polyhexamethylene biguanide hydrochloride is grafted on the surface of silver-loaded magnesium oxide, so that the antibacterial effect of the antibacterial additive can be further improved, and the dispersibility of the silver-loaded magnesium oxide and the stability of the polyhexamethylene biguanide hydrochloride can be improved, so that the antibacterial additive has a long-acting antibacterial effect.
The invention obtains modified polyamide through polycondensation reaction of polyether amine and adipic acid. Because the polyether amine has a flexible chain segment and good water absorption, the prepared modified polyamide has good elasticity, moisture absorption capacity and antistatic capacity. The antibacterial additive is added in the preparation process of the modified polyether amine, so that the carboxyl and the amino which do not participate in the amide reaction on the surface of the antibacterial additive are likely to participate in the polycondensation reaction, and the antibacterial additive is copolymerized on the main chain of the modified polyamide, so that the stability of the antibacterial additive can be further improved, and meanwhile, the antibacterial capability and the antistatic capability of the modified polyamide are improved.
The invention melt-spins the propenyl elastomer, the alkyl quaternary ammonium salt modified montmorillonite, the modified polyamide and the polyamide to obtain the modified nylon filament. Because the propenyl elastomer has high elasticity, the alkyl quaternary ammonium salt modified montmorillonite has antibacterial active groups, and the modified polyamide has better elasticity, antibacterial capability and antistatic capability, the prepared modified nylon filament has high elasticity while having antibacterial and antistatic capabilities.
In addition, the silver-loaded magnesia and alkyl quaternary ammonium salt modified montmorillonite are used as inorganic particles, so that the mechanical properties of the nylon filament are enhanced, and the heat resistance and the wear resistance of the nylon filament can be increased. The nylon filament is coated on the spandex filament, and the prepared nylon-spandex coated yarn has high elasticity, excellent mechanical properties, antibacterial property and antistatic property.
Drawings
FIG. 1 is a process flow diagram of the preparation of a high elasticity nylon-spandex covered yarn of the invention.
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
The embodiment discloses a preparation method of a high-elasticity nylon-spandex coated yarn, which comprises the following steps:
mixing 20wt% of silver nitrate aqueous solution, 20wt% of magnesium nitrate aqueous solution and citric acid, stirring at 80 ℃ for reaction for 4 hours, drying at 130 ℃ for 4 hours after the reaction is finished, heating to 600 ℃ and sintering for 2 hours, wherein the heating rate is 2 ℃/min, and obtaining silver-loaded magnesium oxide; wherein, the mass ratio of the silver nitrate to the magnesium nitrate to the citric acid is 1:10:10; silver-loaded magnesium oxide, 1mol/L hydrochloric acid aqueous solution and water in a mass ratio of 1:3:20, mixing, acidifying at room temperature for 6 hours, filtering after the reaction is finished, adding water with the mass 10 times of that of the silver-loaded magnesium oxide for washing for three times, and drying at 60 ℃ for 24 hours to obtain modified silver-loaded magnesium oxide;
step (2), mixing the modified silver-loaded magnesium oxide with a phosphate buffer solution with a pH value of 5.5 according to a mass ratio of 1:1000, mixing, carrying out ultrasonic treatment for 20min, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, reacting for 2h at the room temperature at the rotating speed of 180r/min, filtering after the reaction is finished, and adding water with the mass of 10 times of that of the modified silver-loaded magnesium oxide for washing to obtain a reaction product; mixing the reaction product with a phosphate buffer solution with a pH value of 7.5 according to a mass ratio of 1:1000, adding 20wt% polyhexamethylene biguanide hydrochloride aqueous solution, continuously reacting for 4 hours at the rotating speed of 180r/min and the room temperature, centrifuging after the reaction is finished, taking the centrifugal precipitate, adding water with the mass 5 times of that of the centrifugal precipitate for three times, and drying for 18 hours at the temperature of 60 ℃ to obtain the antibacterial additive; wherein, the mass ratio of the modified silver-loaded magnesium oxide to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the N-hydroxysuccinimide to the polyhexamethylene biguanide hydrochloride is 1:8:8:10;
dropwise adding polyether amine-ethanol solution into adipic acid-ethanol solution for 30min, adding an antibacterial additive after dropwise adding, reacting for 1h at 50 ℃, filtering after the reaction is finished, and drying for 5h at 60 ℃ to obtain a modified polyamide crude product; mixing the modified polyamide crude product with water in a mass ratio of 3:2, mixing, carrying out a second reaction for 1h in a nitrogen atmosphere at 110 ℃, after the reaction is finished, carrying out a continuous reaction for 4h in the nitrogen atmosphere at 260 ℃, and cooling to room temperature after the reaction is finished to obtain modified polyamide; wherein, the mass ratio of polyetheramine, adipic acid and antibacterial additive is 45:43:5, a step of; the polyetheramine is polyetheramine EDR-148; the polyetheramine-ethanol solution is prepared from polyetheramine and ethanol in a mass ratio of 45:250 are mixed and dissolved to prepare the water-soluble paint; adipic acid-ethanol solution is prepared from adipic acid and ethanol at 45 ℃ in a mass ratio of 43:280 are mixed and dissolved to prepare the catalyst;
step (4), acrylic elastomer, alkyl quaternary ammonium salt modified montmorillonite, modified polyamide and polyamide are mixed according to the mass ratio of 10:3:20:80, melting at 260 ℃, and spinning at a spinning speed of 1500m/min to obtain modified nylon filaments with fineness of 50D; coating the core yarn by using spandex filaments as the core yarn and using modified nylon filaments to obtain high-elasticity nylon-spandex coated yarn; wherein the fineness of the spandex filament is 100D; the coating process comprises the following steps: coating by adopting a ZP-40 ring spinning frame (Shanghai Zhuo Peng Kokoku Co., ltd.), feeding spandex filaments into a roller, pre-drafting by 3 times, and feeding the spandex filaments into a front roller jaw through a godet wheel; the modified nylon filaments are converged with spandex filaments through a rear roller and a middle roller at a front roller, and a covered yarn is formed under the twisting action of a spinning frame, so that the high-elasticity nylon-spandex covered yarn is obtained; the fine spindle speed was 8000RPM and the spun yarn twist factor was 500.
Example 2
The embodiment discloses a preparation method of a high-elasticity nylon-spandex coated yarn, which comprises the following steps:
mixing 20wt% of silver nitrate aqueous solution, 20wt% of magnesium nitrate aqueous solution and citric acid, stirring at 70 ℃ for reaction for 6 hours, drying at 150 ℃ for 2 hours after the reaction is finished, and heating to 600 ℃ for sintering for 2 hours to obtain silver-loaded magnesium oxide; silver-loaded magnesium oxide, 1mol/L hydrochloric acid aqueous solution and water in a mass ratio of 1:1.5:10, mixing, acidizing at room temperature for 12 hours, filtering after the reaction is finished, adding water with the mass of 8 times of that of the silver-loaded magnesium oxide for three times, and drying at 80 ℃ for 12 hours to obtain modified silver-loaded magnesium oxide; wherein, the mass ratio of the silver nitrate to the magnesium nitrate to the citric acid is 0.8:10:10; the temperature rising rate is 5 ℃/min;
step (2), mixing the modified silver-loaded magnesium oxide with a phosphate buffer solution with a pH value of 5.5 according to a mass ratio of 1:800, mixing, carrying out ultrasonic treatment for 30min, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, reacting for 2h at the room temperature at the rotating speed of 200r/min, filtering after the reaction is finished, and adding water with the mass of 8 times of the modified silver-loaded magnesium oxide for washing to obtain a reaction product; mixing the reaction product with a phosphate buffer solution with a pH value of 7.5 according to a mass ratio of 1:800, adding 20wt% polyhexamethylene biguanide hydrochloride aqueous solution, continuously reacting for 6 hours at the rotating speed of 200r/min and the room temperature, centrifuging after the reaction is finished, taking the centrifugal precipitate, adding water with the mass 3 times of that of the centrifugal precipitate for three times, and drying for 24 hours at the temperature of 50 ℃ to obtain the antibacterial additive; wherein, the mass ratio of the modified silver-loaded magnesium oxide to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the N-hydroxysuccinimide to the polyhexamethylene biguanide hydrochloride is 1:10:10:15;
dropwise adding polyether amine-ethanol solution into adipic acid-ethanol solution for 20min, adding an antibacterial additive after dropwise adding, reacting for 2h at 40 ℃, filtering after the reaction is finished, and drying for 8h at 50 ℃ to obtain a modified polyamide crude product; mixing the modified polyamide crude product with water in a mass ratio of 3:2, mixing, carrying out a second reaction for 3 hours at 90 ℃ in a nitrogen atmosphere, after the reaction is finished, carrying out a continuous reaction for 6 hours at 250 ℃ in the nitrogen atmosphere, and cooling to room temperature after the reaction is finished to obtain modified polyamide; wherein, the mass ratio of polyetheramine, adipic acid and antibacterial additive is 45:43:4, a step of; the polyetheramine is polyetheramine EDR-148; the polyetheramine-ethanol solution is prepared from polyetheramine and ethanol in a mass ratio of 50:320, mixing and dissolving to prepare the material; adipic acid-ethanol solution is prepared from adipic acid and ethanol at 45 ℃ in a mass ratio of 50:340 is prepared by mixing and dissolving;
step (4), acrylic elastomer, alkyl quaternary ammonium salt modified montmorillonite, modified polyamide and polyamide are mixed according to the mass ratio of 8:3:18:85, melting at 220 ℃, and spinning at a spinning speed of 3200m/min to obtain modified nylon filaments with fineness of 120D; coating the core yarn by using spandex filaments as the core yarn and using modified nylon filaments to obtain high-elasticity nylon-spandex coated yarn; wherein the fineness of the spandex filament is 60D; the cladding process was the same as in example 1.
Example 3
The embodiment discloses a preparation method of a high-elasticity nylon-spandex coated yarn, which comprises the following steps:
mixing 20wt% of silver nitrate aqueous solution, 20wt% of magnesium nitrate aqueous solution and citric acid, stirring at 75 ℃ for reaction for 5 hours, drying at 140 ℃ for 3 hours after the reaction is finished, and heating to 600 ℃ for sintering for 2 hours to obtain silver-loaded magnesium oxide; silver-loaded magnesium oxide, 1mol/L hydrochloric acid aqueous solution and water in a mass ratio of 1:2:15, mixing, acidifying at room temperature for 10 hours, filtering after the reaction is finished, adding water with the mass 9 times of that of the silver-loaded magnesium oxide for three times, and drying at 70 ℃ for 18 hours to obtain modified silver-loaded magnesium oxide; wherein, the mass ratio of the silver nitrate to the magnesium nitrate to the citric acid is 0.5:10:9, a step of performing the process; the temperature rising rate is 4 ℃/min;
step (2), mixing the modified silver-loaded magnesium oxide with a phosphate buffer solution with a pH value of 5.5 according to a mass ratio of 1:900, mixing, carrying out ultrasonic treatment for 25min, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, reacting for 2h at the room temperature at the rotating speed of 190r/min, filtering after the reaction is finished, and adding water with the mass of 9 times of that of the modified silver-loaded magnesium oxide for washing to obtain a reaction product; mixing the reaction product with a phosphate buffer solution with a pH value of 7.5 according to a mass ratio of 1:900, adding 20wt% polyhexamethylene biguanide hydrochloride aqueous solution, continuously reacting for 5 hours at the rotating speed of 190r/min and the room temperature, centrifuging after the reaction is finished, taking the centrifugal precipitate, adding water with the mass 4 times of that of the centrifugal precipitate for three times, and drying for 20 hours at the temperature of 55 ℃ to obtain the antibacterial additive; wherein, the mass ratio of the modified silver-loaded magnesium oxide to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the N-hydroxysuccinimide to the polyhexamethylene biguanide hydrochloride is 1:9:9:12;
dropwise adding polyether amine-ethanol solution into adipic acid-ethanol solution for 25min, adding an antibacterial additive after dropwise adding, reacting for 1.5h at 45 ℃, filtering after the reaction is finished, and drying for 7h at 55 ℃ to obtain a modified polyamide crude product; mixing the modified polyamide crude product with water in a mass ratio of 3:2, mixing, carrying out a second reaction for 2 hours at 100 ℃ in a nitrogen atmosphere, after the reaction is finished, carrying out a continuous reaction for 5 hours at 255 ℃ in the nitrogen atmosphere, and cooling to room temperature after the reaction is finished to obtain modified polyamide; wherein, the mass ratio of polyetheramine, adipic acid and antibacterial additive is 45:43:3, a step of; the polyetheramine is polyetheramine EDR-148; the polyetheramine-ethanol solution is prepared from polyetheramine and ethanol in a mass ratio of 48:280 are mixed and dissolved to prepare the catalyst; adipic acid-ethanol solution is prepared from adipic acid and ethanol at 45 ℃ in a mass ratio of 45:300 is prepared by mixing and dissolving;
step (4), acrylic elastomer, alkyl quaternary ammonium salt modified montmorillonite, modified polyamide and polyamide are mixed according to the mass ratio of 7:3:15:90, melting at 240 ℃, and spinning at a spinning speed of 2500m/min to obtain modified nylon filaments with fineness of 70D; coating the core yarn by using spandex filaments as the core yarn and using modified nylon filaments to obtain high-elasticity nylon-spandex coated yarn; wherein the fineness of the spandex filament is 80D; the cladding process was the same as in example 1.
Example 4
The embodiment discloses a preparation method of a high-elasticity nylon-spandex coated yarn, which comprises the following steps:
mixing 20wt% of silver nitrate aqueous solution, 20wt% of magnesium nitrate aqueous solution and citric acid, stirring at 72 ℃ for reaction for 5.5 hours, drying at 135 ℃ for 4 hours after the reaction is finished, and heating to 600 ℃ for sintering for 2 hours to obtain silver-loaded magnesium oxide; silver-loaded magnesium oxide, 1mol/L hydrochloric acid aqueous solution and water in a mass ratio of 1:2.5:20, mixing, acidizing at room temperature for 8 hours, filtering after the reaction is finished, adding water with the mass 10 times of that of the silver-loaded magnesium oxide for washing for three times, and drying at 65 ℃ for 20 hours to obtain modified silver-loaded magnesium oxide; wherein, the mass ratio of the silver nitrate to the magnesium nitrate to the citric acid is 0.3:10:8, 8; the temperature rising rate is 3 ℃/min;
step (2), mixing the modified silver-loaded magnesium oxide with a phosphate buffer solution with a pH value of 5.5 according to a mass ratio of 1:800, mixing, carrying out ultrasonic treatment for 20min, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, reacting for 2h at the room temperature at the rotating speed of 180r/min, filtering after the reaction is finished, and adding water with the mass of 10 times of that of the modified silver-loaded magnesium oxide for washing to obtain a reaction product; mixing the reaction product with a phosphate buffer solution with a pH value of 7.5 according to a mass ratio of 1:1000, adding 20wt% polyhexamethylene biguanide hydrochloride aqueous solution, continuously reacting for 5 hours at the rotating speed of 200r/min and the room temperature, centrifuging after the reaction is finished, taking the centrifugal precipitate, adding water with the mass 5 times of that of the centrifugal precipitate for three times, and drying for 18 hours at the temperature of 60 ℃ to obtain the antibacterial additive; wherein, the mass ratio of the modified silver-loaded magnesium oxide to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the N-hydroxysuccinimide to the polyhexamethylene biguanide hydrochloride is 1:10:10:13;
dropwise adding polyether amine-ethanol solution into adipic acid-ethanol solution for 30min, adding an antibacterial additive after dropwise adding, reacting for 2h at 40 ℃, filtering after the reaction is finished, and drying for 5h at 60 ℃ to obtain a modified polyamide crude product; mixing the modified polyamide crude product with water in a mass ratio of 3:2, mixing, carrying out a second reaction for 2.5 hours at the temperature of 95 ℃ in a nitrogen atmosphere, after the reaction is finished, carrying out a continuous reaction for 6 hours at the temperature of 250 ℃ in the nitrogen atmosphere, and cooling to room temperature after the reaction is finished to obtain modified polyamide; wherein, the mass ratio of polyetheramine, adipic acid and antibacterial additive is 45:43:2; the polyetheramine is polyetheramine EDR-148; the polyetheramine-ethanol solution is prepared from polyetheramine and ethanol in a mass ratio of 50:300 is prepared by mixing and dissolving; adipic acid-ethanol solution is prepared from adipic acid and ethanol at 45 ℃ in a mass ratio of 48:340 is prepared by mixing and dissolving;
step (4), acrylic elastomer, alkyl quaternary ammonium salt modified montmorillonite, modified polyamide and polyamide are mixed according to the mass ratio of 6:2:13:95, melting at 250 ℃, and spinning at a spinning speed of 2000m/min to obtain modified nylon filaments with fineness of 80D; coating the core yarn by using spandex filaments as the core yarn and using modified nylon filaments to obtain high-elasticity nylon-spandex coated yarn; wherein the fineness of the spandex filament is 70D; the cladding process was the same as in example 1.
Example 5
The embodiment discloses a preparation method of a high-elasticity nylon-spandex coated yarn, which comprises the following steps:
mixing 20wt% of silver nitrate aqueous solution, 20wt% of magnesium nitrate aqueous solution and citric acid, stirring at 80 ℃ for reaction for 4 hours, drying at 135 ℃ for 4 hours after the reaction is finished, and heating to 600 ℃ for sintering for 2 hours to obtain silver-loaded magnesium oxide; silver-loaded magnesium oxide, 1mol/L hydrochloric acid aqueous solution and water in a mass ratio of 1:2.5:20, mixing, acidifying at room temperature for 10 hours, filtering after the reaction is finished, adding water with the mass 10 times of that of the silver-loaded magnesium oxide for washing for three times, and drying at 75 ℃ for 16 hours to obtain modified silver-loaded magnesium oxide; wherein, the mass ratio of the silver nitrate to the magnesium nitrate to the citric acid is 0.1:10:8, 8; the temperature rising rate is 5 ℃/min;
step (2), mixing the modified silver-loaded magnesium oxide with a phosphate buffer solution with a pH value of 5.5 according to a mass ratio of 1:850, mixing, carrying out ultrasonic treatment for 30min, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, reacting for 2h at the room temperature at the rotating speed of 200r/min, filtering after the reaction is finished, and adding water with the mass of 8 times of the modified silver-loaded magnesium oxide for washing to obtain a reaction product; mixing the reaction product with a phosphate buffer solution with a pH value of 7.5 according to a mass ratio of 1:1000, adding 20wt% polyhexamethylene biguanide hydrochloride aqueous solution, continuously reacting for 6 hours at the rotating speed of 180r/min and the room temperature, centrifuging after the reaction is finished, taking the centrifugal precipitate, adding water with the mass 3 times of that of the centrifugal precipitate for three times, and drying for 24 hours at the temperature of 50 ℃ to obtain the antibacterial additive; wherein, the mass ratio of the modified silver-loaded magnesium oxide to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the N-hydroxysuccinimide to the polyhexamethylene biguanide hydrochloride is 1:8:8:10;
dropwise adding polyether amine-ethanol solution into adipic acid-ethanol solution for 20min, adding an antibacterial additive after dropwise adding, reacting for 1h at 50 ℃, filtering after the reaction is finished, and drying for 7h at 50 ℃ to obtain a modified polyamide crude product; mixing the modified polyamide crude product with water in a mass ratio of 3:2, mixing, carrying out a second reaction for 1.5 hours at 105 ℃ in a nitrogen atmosphere, after the reaction is finished, carrying out a continuous reaction for 4 hours at 260 ℃ in the nitrogen atmosphere, and cooling to room temperature after the reaction is finished, thus obtaining modified polyamide; wherein, the mass ratio of polyetheramine, adipic acid and antibacterial additive is 45:43:1, a step of; the polyetheramine is polyetheramine EDR-148; the polyetheramine-ethanol solution is prepared from polyetheramine and ethanol in a mass ratio of 50:280 are mixed and dissolved to prepare the catalyst; adipic acid-ethanol solution is prepared from adipic acid and ethanol at 45 ℃ in a mass ratio of 43:300 is prepared by mixing and dissolving;
step (4), acrylic elastomer, alkyl quaternary ammonium salt modified montmorillonite, modified polyamide and polyamide are mixed according to the mass ratio of 5:2:10:100, melting at 260 ℃, and spinning at a spinning speed of 3000m/min to obtain modified nylon filaments with fineness of 60D; coating the core yarn by using spandex filaments as the core yarn and using modified nylon filaments to obtain high-elasticity nylon-spandex coated yarn; wherein the fineness of the spandex filament is 100D; the cladding process was the same as in example 1.
Comparative example 1
The comparative example discloses a preparation method of a high-elasticity nylon-spandex coated yarn, which comprises the following steps:
dropwise adding polyether amine-ethanol solution into adipic acid-ethanol solution for 30min, reacting for 1h at 50 ℃ after dropwise adding, filtering after the reaction is finished, and drying for 5h at 60 ℃ to obtain a modified polyamide crude product; mixing the modified polyamide crude product with water in a mass ratio of 3:2, mixing, carrying out a second reaction for 1h in a nitrogen atmosphere at 110 ℃, after the reaction is finished, carrying out a continuous reaction for 4h in the nitrogen atmosphere at 260 ℃, and cooling to room temperature after the reaction is finished to obtain modified polyamide; wherein, the mass ratio of polyetheramine to adipic acid is 47:46; the polyetheramine is polyetheramine EDR-148; the polyetheramine-ethanol solution is prepared from polyetheramine and ethanol in a mass ratio of 45:250 are mixed and dissolved to prepare the water-soluble paint; adipic acid-ethanol solution is prepared from adipic acid and ethanol at 45 ℃ in a mass ratio of 43:280 are mixed and dissolved to prepare the catalyst;
step (2), propylene-based elastomer, polyhexamethylene biguanide hydrochloride, modified polyamide and polyamide are mixed according to the mass ratio of 10:3:20:80, melting at 260 ℃, and spinning at a spinning speed of 1500m/min to obtain modified nylon filaments with fineness of 50D; coating the core yarn by using spandex filaments as the core yarn and using modified nylon filaments to obtain high-elasticity nylon-spandex coated yarn; wherein the fineness of the spandex filament is 100D; the cladding process was the same as in example 1.
Comparative example 2
The comparative example discloses a preparation method of a high-elasticity nylon-spandex coated yarn, which comprises the following steps:
mixing 20wt% of silver nitrate aqueous solution, 20wt% of magnesium nitrate aqueous solution and citric acid, stirring at 80 ℃ for reaction for 4 hours, drying at 130 ℃ for 4 hours after the reaction is finished, and heating to 600 ℃ for sintering for 2 hours to obtain silver-loaded magnesium oxide; silver-loaded magnesium oxide, 1mol/L hydrochloric acid aqueous solution and water in a mass ratio of 1:3:20, mixing, acidifying at room temperature for 6 hours, filtering after the reaction is finished, adding water with the mass 10 times of that of the silver-loaded magnesium oxide for washing for three times, and drying at 60 ℃ for 24 hours to obtain modified silver-loaded magnesium oxide; wherein, the mass ratio of the silver nitrate to the magnesium nitrate to the citric acid is 1:10:10; the temperature rising rate is 2 ℃/min;
step (2), mixing the modified silver-loaded magnesium oxide with a phosphate buffer solution with a pH value of 5.5 according to a mass ratio of 1:1000, mixing, carrying out ultrasonic treatment for 20min, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, reacting for 2h at the room temperature at the rotating speed of 180r/min, filtering after the reaction is finished, and adding water with the mass of 10 times of that of the modified silver-loaded magnesium oxide for washing to obtain a reaction product; mixing the reaction product with a phosphate buffer solution with a pH value of 7.5 according to a mass ratio of 1:1000, adding 20wt% polyhexamethylene biguanide hydrochloride aqueous solution, continuously reacting for 4 hours at the rotating speed of 180r/min and the room temperature, centrifuging after the reaction is finished, taking the centrifugal precipitate, adding water with the mass 5 times of that of the centrifugal precipitate for three times, and drying for 18 hours at the temperature of 60 ℃ to obtain the antibacterial additive; wherein, the mass ratio of the modified silver-loaded magnesium oxide to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the N-hydroxysuccinimide to the polyhexamethylene biguanide hydrochloride is 1:8:8:10;
step (3), alkyl quaternary ammonium salt modified montmorillonite, an antibacterial additive and polyamide in a mass ratio of 3:1:110, melting at 260 ℃, and spinning at a spinning speed of 1500m/min to obtain modified nylon filaments with fineness of 50D; coating the core yarn by using spandex filaments as the core yarn and using modified nylon filaments to obtain high-elasticity nylon-spandex coated yarn; wherein the fineness of the spandex filament is 100D; the cladding process was the same as in example 1.
Comparative example 3
The comparative example discloses a preparation method of a high-elasticity nylon-spandex coated yarn, which comprises the following steps: propylene elastomer, alkyl quaternary ammonium salt modified montmorillonite and polyamide are mixed according to the mass ratio of 10:3:100, melting at 260 ℃, and spinning at a spinning speed of 1500m/min to obtain modified nylon filaments with fineness of 50D; coating the core yarn by using spandex filaments as the core yarn and using modified nylon filaments to obtain high-elasticity nylon-spandex coated yarn; wherein the fineness of the spandex filament is 100D; the cladding process was the same as in example 1.
In the above examples and comparative examples: silver nitrate was obtained from sigma aldrich trade limited, cat No. 204390, cas No.: 7761-88-8; citric acid from Jinan flag is chemical industry Co., ltd., model analysis pure, CAS number: 77-92-9; the aqueous hydrochloric acid solution is from Shanghai Yuan Ye Biotechnology Co., ltd., product number B62243, model hydrogen chloride standard solution; phosphate buffer from the company of Itembotu Biotechnology, inc., named PBS phosphate buffer; 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride from the international trade company, pandalton (Shanghai), CAS number: 25952-53-8; n-hydroxysuccinimide was from Hubei Jiahuixing Chengcheng Biotechnology Co., ltd., CAS number: 6066-82-6; polyhexamethylene biguanide hydrochloride is available from the company Tianjin, mitsui environmental protection technology, inc., model powder, CAS number: 32289-58-0; ethanol is from Shanghai Poisson chemical Co., ltd., CAS number: 64-17-5; adipic acid was obtained from medal chemical company, model analytically pure, CAS number: 124-04-9; polyetheramine is from Shinewgeneral Ming Chemie (Shanghai) Inc., brand Hensmai, model polyetheramine EDR-148; the propylene-based elastomer is from the company ExxonMobil, under the brand vistamaxx6102; alkyl quaternary ammonium salt modified montmorillonite is from Zhejiang Huate new materials limited company, and the product number is DK-2; the polyamide is from the company Dongguan, polyron plastics materials, inc., brand German Basiff, model B27N02.
Test examples
(1) Testing of mechanical Properties and antistatic Properties
The mechanical properties and antistatic properties of the high-elasticity nylon-spandex coated yarns prepared in examples 1 to 5 and comparative examples 1 to 3 were tested, and specific test results are shown in table 1:
the detection of each index in table 1 is based on the following criteria: the elastic recovery degree is measured by FZ/T50007-2012 spandex silk elasticity test method; the breaking strength and the breaking elongation are determined by GB/T3916-2013 (determination of breaking strength and breaking elongation of textile, package yarn, individual yarn (CRE method)); the surface resistance is measured by GB/T22042-2008 clothing antistatic property surface resistivity test method.
According to the test results of Table 1, it can be seen that the high-elasticity nylon-spandex coated yarn prepared by the method has high elasticity, antistatic capability and excellent mechanical properties, and has wide application prospects in fabrics.
In comparative example 1, no antibiotic additive and alkyl quaternary ammonium salt modified montmorillonite are added, and since both magnesium oxide and silver in the antibiotic additive have conductivity and silver is doped in magnesium oxide crystals, a network for transferring electrons is formed, and leakage of charges is accelerated, the nylon added with the antibiotic additive has antistatic capability. The comparative example 1 lacks the effect of enhancing the mechanical property and antistatic ability of the nylon filaments by using the conductive particles-loaded silver magnesium oxide and the alkyl quaternary ammonium salt modified montmorillonite as inorganic particles, so that the surface resistance of the comparative example 1 is higher than that of the examples, the breaking strength is lower than that of the examples, and the mechanical property and antistatic ability are inferior to those of the examples; in comparative example 2, no acryl elastomer and modified polyamide were added, and the polyether amine had a soft segment and good water absorption, so that the prepared modified polyamide had good elasticity, moisture absorption capacity and antistatic ability. The antibacterial additive is added in the preparation process of the modified polyether amine, so that the carboxyl and amino which do not participate in the amide reaction are likely to participate in the polycondensation reaction on the surface of the antibacterial additive, and the antibacterial additive is copolymerized on the main chain of the modified polyamide, so that the stability of the antibacterial additive can be further improved, and the antistatic capability of the modified polyamide is improved. The comparative example 2 lacks the antistatic ability of the modified polyamide and the propylene-based elastomer has high elastic action, but the antistatic property of the comparative example 2 is still inferior to that of the example, and the elastic recovery degree is lower than that of the example, although the silver-loaded magnesium oxide in the antibacterial additive has the conductive effect; comparative example 3, in which the antibiotic additive and the modified polyamide were not added, lacks the antistatic ability of the modified polyamide and the conductive ability of silver-loaded magnesium oxide in the antibiotic additive, so that the antistatic property is lower than that of the example.
(2) Antibacterial property test
The antibacterial properties of the high elastic nylon-spandex coated yarns prepared in examples 1 to 5 and comparative examples 1 to 3 were tested, and specific test results are shown in table 2:
table 2 the detection of each index is based on the following criteria: the antibacterial rate is evaluated by GB/T20944.3-2008 section 3 of antibacterial Properties of textiles: the method of vibration.
As can be seen from the test results in Table 2, the high-elasticity nylon-spandex coated yarn prepared by the method has excellent antibacterial property and has wide application prospects in fabrics.
In comparative example 1, no antibacterial additive and alkyl quaternary ammonium salt modified montmorillonite are added, polyhexamethylene guanidine is used as an antibacterial agent to be added into modified nylon filaments, and as silver-loaded magnesia has excellent antibacterial capability, carboxyl groups on the surface and terminal amino groups of polyhexamethylene biguanide hydrochloride are subjected to amidation reaction through acidizing the surface of the silver-loaded magnesia, so that an organic antibacterial agent can be grafted on the surface of the silver-loaded magnesia, the antibacterial effect of the antibacterial additive can be further improved, and the dispersibility of the silver-loaded magnesia and the stability of polyhexamethylene biguanide hydrochloride can be improved, so that the antibacterial additive has a long-acting antibacterial effect. The alkyl quaternary ammonium salt modified montmorillonite has antibacterial active groups, so that the montmorillonite has antibacterial property. In comparative example 1, even though polyhexamethylene guanidine has a certain antibacterial property due to the lack of an antibacterial additive and the antibacterial ability of alkyl quaternary ammonium salt modified montmorillonite, the polyhexamethylene guanidine has insufficient stability in a matrix, and the antibacterial effect is affected, so that the antibacterial rate is lower than that of the examples; in comparative example 3, no antibiotic additive and modified polyamide were added, and the antibacterial efficiency was lower than in example, although the alkyl quaternary ammonium salt modified montmorillonite still had an antibacterial effect due to the lack of the antibacterial ability of the antibacterial agent.
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 high-elasticity nylon-spandex coated yarn is characterized by comprising the following steps of:
step (1), mixing silver nitrate aqueous solution, magnesium nitrate aqueous solution and citric acid, reacting, drying after the reaction is finished, and sintering to obtain silver-loaded magnesium oxide; mixing silver-loaded magnesia, hydrochloric acid aqueous solution and water, carrying out acidification reaction, filtering, washing and drying after the reaction is finished to obtain modified silver-loaded magnesia;
step (2), mixing the modified silver-loaded magnesium oxide with a phosphate buffer solution, performing ultrasound, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, reacting, filtering after the reaction is finished, and washing to obtain a reaction product; mixing the reaction product with a phosphate buffer solution, adding a polyhexamethylene biguanide hydrochloride aqueous solution, continuing to react, centrifuging after the reaction is finished, taking a centrifugal precipitate, washing, and drying to obtain an antibacterial additive;
step (3), dropwise adding polyether amine-ethanol solution into adipic acid-ethanol solution, adding an antibacterial additive after dropwise adding, carrying out a first reaction, filtering after the reaction is finished, and drying to obtain a modified polyamide crude product; mixing the modified polyamide crude product with water, carrying out a second reaction, continuing the reaction after the reaction is finished, and cooling after the reaction is finished to obtain modified polyamide;
step (4), mixing the propenyl elastomer, the alkyl quaternary ammonium salt modified montmorillonite, the modified polyamide and the polyamide, and carrying out melt spinning to obtain modified nylon filaments; and coating the core yarn by using the spandex filaments as the core yarn and using modified nylon filaments to obtain the high-elasticity nylon-spandex coated yarn.
2. The method for producing a high elastic nylon-spandex covered yarn according to claim 1, wherein in the step (1): the mass ratio of the silver nitrate to the magnesium nitrate to the citric acid is (0.1-1): 10: (8-10); the reaction conditions are as follows: stirring and reacting for 4-6h at 70-80 ℃; the drying conditions are as follows: drying at 130-150deg.C for 2-4 hr; the sintering conditions are as follows: heating to 600 ℃ and sintering for 2 hours, wherein the heating rate is 2-5 ℃/min.
3. The method for producing a high elastic nylon-spandex covered yarn according to claim 1, wherein in the step (1): the mass ratio of the silver-loaded magnesium oxide to the hydrochloric acid aqueous solution to the water is 1: (1.5-3): (10-20); the acidification reaction conditions are as follows: acidizing reaction at room temperature for 6-12h.
4. The method for producing a high-elasticity nylon-spandex covered yarn according to claim 1, wherein in the step (2): the mass ratio of the modified silver-carrying magnesium oxide to the phosphate buffer solution is 1: (800-1000); the reaction conditions are as follows: reacting for 2 hours at room temperature at the rotating speed of 180-200 r/min; the mass ratio of the reaction product to the phosphate buffer solution is 1: (800-1000); the continuous reaction conditions are as follows: continuously reacting for 4-6h at room temperature at the rotating speed of 180-200 r/min; the pH value of the phosphate buffer solution mixed with the modified silver-carrying magnesium oxide is 5.5; the pH of the phosphate buffer solution mixed with the reaction product was 7.5.
5. The method for producing a high-elasticity nylon-spandex covered yarn according to claim 1, wherein in the step (2): the mass ratio of the modified silver-loaded magnesium oxide to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the N-hydroxysuccinimide to the polyhexamethylene biguanide hydrochloride is 1: (8-10): (8-10): (10-15).
6. The method for producing a high-elasticity nylon-spandex covered yarn according to claim 1, wherein in the step (3): the mass ratio of polyetheramine, adipic acid and the antibacterial additive is 45:43: (1-5); the dropping conditions are as follows: dripping at room temperature for 20-30min; the first reaction conditions are as follows: reacting for 1-2h at 40-50 ℃; the mass ratio of the modified polyamide crude product to water is 3:2; the second reaction conditions are as follows: reacting for 1-3h in nitrogen atmosphere at 90-110 ℃; the continuous reaction conditions are as follows: and continuing the reaction for 4-6h at the temperature of 250-260 ℃ in a nitrogen atmosphere.
7. The method for producing a high-elasticity nylon-spandex covered yarn according to claim 1, wherein in the step (4): the mass ratio of the propenyl elastomer to the alkyl quaternary ammonium salt modified montmorillonite to the modified polyamide to the polyamide is (5-10): (2-3): (10-20): (80-100); the melt spinning conditions are: melting at 220-260 deg.C, spinning at 1500-3200 m/min.
8. The method for producing a high-elasticity nylon-spandex covered yarn according to claim 1, wherein in the step (4): the fineness of the modified nylon filament is 50-120D; the fineness of the spandex filament is 60-100D.
9. A high-elasticity nylon-spandex covered yarn prepared by the method for preparing a high-elasticity nylon-spandex covered yarn according to any one of claims 1 to 8.
10. Use of the high-elasticity nylon-spandex covered yarn according to claim 9 in a fabric.
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Non-Patent Citations (3)
| Title |
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| 朱正宇等: "《功率半导体器件封装技术》", vol. 1, 31 August 2022, 机械工业出版社, pages: 54 - 59 * |
| 汪多仁: "《绿色增塑剂》", vol. 1, 31 October 2011, 科学技术文献出版社, pages: 423 - 424 * |
| 王绍荣等: "《固体氧化物燃料电池 吃粗粮的大力士》", vol. 1, 30 June 2013, 武汉大学出版社, pages: 60 - 61 * |
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