CN113527850A - Cool functional masterbatch, cool fiber and preparation method and application thereof - Google Patents
Cool functional masterbatch, cool fiber and preparation method and application thereof Download PDFInfo
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- CN113527850A CN113527850A CN202110937183.XA CN202110937183A CN113527850A CN 113527850 A CN113527850 A CN 113527850A CN 202110937183 A CN202110937183 A CN 202110937183A CN 113527850 A CN113527850 A CN 113527850A
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- jade
- crystal jade
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- 239000000835 fiber Substances 0.000 title claims abstract description 109
- 239000004594 Masterbatch (MB) Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000010977 jade Substances 0.000 claims abstract description 75
- 239000013078 crystal Substances 0.000 claims abstract description 58
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000009830 intercalation Methods 0.000 claims abstract description 25
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000005342 ion exchange Methods 0.000 claims abstract description 17
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 11
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims description 37
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 17
- 238000002074 melt spinning Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 12
- 238000009987 spinning Methods 0.000 claims description 12
- 239000011787 zinc oxide Substances 0.000 claims description 12
- 239000003963 antioxidant agent Substances 0.000 claims description 11
- 230000003078 antioxidant effect Effects 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 238000012986 modification Methods 0.000 claims description 10
- 230000004048 modification Effects 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 9
- 239000011347 resin Substances 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 9
- 238000005520 cutting process Methods 0.000 claims description 8
- 238000001125 extrusion Methods 0.000 claims description 8
- 239000004753 textile Substances 0.000 claims description 5
- 238000004804 winding Methods 0.000 claims description 5
- 229910001610 cryolite Inorganic materials 0.000 claims description 4
- 238000007493 shaping process Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 15
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 10
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 10
- 239000000377 silicon dioxide Substances 0.000 abstract description 8
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 230000036571 hydration Effects 0.000 abstract description 6
- 238000006703 hydration reaction Methods 0.000 abstract description 6
- 229910001414 potassium ion Inorganic materials 0.000 abstract description 6
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 5
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 4
- 230000032798 delamination Effects 0.000 abstract description 4
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 3
- 125000000524 functional group Chemical group 0.000 abstract description 3
- 230000001737 promoting effect Effects 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 239000011701 zinc Substances 0.000 abstract description 3
- 229910052725 zinc Inorganic materials 0.000 abstract description 3
- 239000002657 fibrous material Substances 0.000 abstract description 2
- 230000003385 bacteriostatic effect Effects 0.000 description 8
- 230000002687 intercalation Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- -1 polyethylene terephthalate Polymers 0.000 description 7
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- 239000005020 polyethylene terephthalate Substances 0.000 description 7
- 230000006750 UV protection Effects 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 5
- 239000004744 fabric Substances 0.000 description 5
- 229920000728 polyester Polymers 0.000 description 5
- 239000004952 Polyamide Substances 0.000 description 4
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 229920002647 polyamide Polymers 0.000 description 4
- 230000017525 heat dissipation Effects 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 241000222122 Candida albicans Species 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 229920002292 Nylon 6 Polymers 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 229940095731 candida albicans Drugs 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 229920001707 polybutylene terephthalate Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 230000004224 protection Effects 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 235000012438 extruded product Nutrition 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 229920006149 polyester-amide block copolymer Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229940113115 polyethylene glycol 200 Drugs 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
- 229940057977 zinc stearate Drugs 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- 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
- 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
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
-
- 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
- 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
- D01F6/92—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 polyesters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Artificial Filaments (AREA)
Abstract
The invention belongs to the technical field of chemical fiber materials, and particularly relates to a cool functional master batch, a cool fiber, and preparation methods and applications thereof. According to the invention, the crystal jade is mixed with lithium nitrate to carry out hydrothermal ion exchange reaction, lithium ions replace potassium ions between crystal jade sheets, and meanwhile, under the hydrothermal ion exchange reaction of a water phase, the lithium ions coat a hydration film, the hydration radius of the lithium ions is greater than that of the potassium ions, so that the aim of promoting the delamination of silicon dioxide sheets of the crystal jade is achieved, and the nano-intercalation crystal jade with charges, high adsorption force, super-hydrophilicity, moisture absorption and cool feeling effect is obtained; the nano-intercalation crystal jade, the sulfuric acid, the nitric acid and the potassium permanganate are mixed, so that the nano-intercalation crystal jade can generate-COOH functional groups, a multi-layer and stable zinc ion-silicon dioxide grafting structure can be formed, the ultraviolet reflection performance of the modified crystal jade can be improved, and the cold master batch with the cold, antibacterial and uvioresistant performances can be obtained.
Description
Technical Field
The invention belongs to the technical field of chemical fiber materials, and particularly relates to a cool functional master batch, a cool fiber, and preparation methods and applications thereof.
Background
The cool fiber is a fiber which can prevent discomfort when wet and has excellent cool feeling when in contact with the skin, and is produced by adding a medium having a low heat absorption rate and a high heat dissipation rate in nature to a carrier such as polyester, nylon, or regenerated cellulose fiber, and thus a woven fabric has excellent cool feeling when in contact with the skin. The common process is to mix the cool factor (i.e. the medium with slow heat absorption speed and fast heat dissipation speed) and the carrier, and prepare the obtained cool functional master batch into cool fiber.
At present, common cool feeling fibers (such as jade fibers and synthetic aluminum nitride fibers) in the market absorb heat quickly and dissipate heat quickly, and when the cool feeling fibers are made into clothes to be worn, the clothes feel cool at the first time, but the temperature of the clothes also rises slowly along with the prolonging of wearing time, the cool feeling effect is lost, and the cool feeling effect is not good enough.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a cool functional masterbatch, and a cool fiber prepared from the cool functional masterbatch provided by the present invention has the characteristics of excellent instantaneous cool feeling and long cool feeling lasting time.
In order to achieve the purpose of the invention, the invention provides the following technical scheme:
the invention provides a preparation method of a cool functional master batch, which comprises the following steps:
mixing the crystal jade with lithium nitrate, and carrying out hydrothermal ion exchange reaction to obtain nano-intercalation crystal jade;
mixing the nano-intercalation crystal jade, sulfuric acid, nitric acid and potassium permanganate, mixing the obtained mixture with zinc oxide, and modifying to obtain modified crystal jade;
and mixing the modified crystal jade, the resin carrier, the dispersing agent and the antioxidant, and performing melt blending and extrusion to obtain the cool functional master batch.
Preferably, the temperature of the hydrothermal ion exchange reaction is 150-180 ℃, and the pressure is 0.35-0.5 MPa.
Preferably, the modification temperature is 150-180 ℃, and the modification time is 3-6 h.
Preferably, the particle size of the modified crystal jade is 100-200 nm.
The invention also provides the cool feeling functional master batch prepared by the preparation method of the technical scheme.
The invention also provides cool fiber which comprises cool fiber filament or cool fiber short fiber, and the preparation material of the cool fiber comprises the cool functional master batch.
Preferably, the monofilament fineness of the cool fiber is 0.8-3.33 dtex.
The invention also provides a preparation method of the cool fiber in the technical scheme, and when the cool fiber is a cool fiber filament, the preparation method of the cool fiber filament comprises the following steps:
mixing the cool functional master batch with the carrier slice, and spinning by a melting method to obtain pre-oriented yarn;
and (3) texturing the pre-oriented yarn to obtain the cool fiber filament.
The invention also provides a preparation method of the cool fiber in the technical scheme, and when the cool fiber is cool fiber short fiber, the preparation method of the cool fiber short fiber comprises the following steps:
mixing the cool functional master batch with the carrier slice, carrying out melt spinning, and winding, molding and bundling the obtained fiber yarn to obtain raw yarn;
and sequentially carrying out subsequent drafting, shaping, curling and cutting on the protofilament to obtain the cool fiber staple fiber.
The invention also provides application of the cool fiber in the technical scheme or the cool fiber prepared by the preparation method in the technical scheme in cool textiles.
The invention provides a preparation method of a cool functional master batch, which comprises the following steps: mixing the crystal jade with lithium nitrate, and carrying out hydrothermal ion exchange reaction to obtain nano-intercalation crystal jade; mixing the nanometer intercalation crystal jade, sulfuric acid and sodium nitrateMixing acid and potassium permanganate, mixing the obtained mixture with zinc oxide, and modifying to obtain modified crystal jade; and mixing the modified crystal jade, the resin carrier, the dispersing agent and the antioxidant, and performing melt blending and extrusion to obtain the cool functional master batch. In the invention, the ice jade has the characteristics of slow heat absorption and fast heat dissipation, and is beneficial to providing excellent cool feeling; mixing the crystal jade with lithium nitrate, carrying out hydrothermal ion exchange reaction, replacing potassium ions between crystal jade sheets with lithium ions, simultaneously coating a layer of hydration film with the lithium ions under the hydrothermal ion exchange reaction of a water phase, wherein the hydration radius of the lithium ions is larger than that of the potassium ions, so as to achieve the purpose of promoting the delamination of the silicon dioxide sheets of the crystal jade, further dispersing the silicon dioxide powder of the crystal jade after the delamination modification, reducing the particle size, grafting the lithium ions on the silicon dioxide sheets, and obtaining the nano intercalation crystal jade with charges, high adsorption force, super-hydrophilicity, moisture absorption and cool feeling effect; the nano-intercalation sparkling jade, the sulfuric acid, the nitric acid and the potassium permanganate are mixed, so that the nano-intercalation sparkling jade can generate a-COOH functional group, then the introduced zinc oxide generates zinc ions, and the zinc ions are combined with the-COOH on the nano-intercalation sparkling jade, a multi-layer and stable zinc ion-silicon dioxide grafting structure can be formed, the ultraviolet reflection performance of the modified sparkling jade can be improved, and the cool master batch with cool feeling, antibacterial performance and ultraviolet resistance can be obtained. The silicon dioxide structure of the lamellar structure of the modified crystal jade enables heat to be rapidly conducted along the lamellar structure, so that the heat conductivity coefficient of the fiber is obviously improved; meanwhile, the laminated structure of the material layers enables the material to have a high thermal diffusion coefficient which reaches 10-4M2(ordinary rock thermal diffusivity is about 10)-6M2And/s, the thermal diffusion coefficient of the modified ice jade is two orders of magnitude higher than that of common rock), so that the temperature rise of the master batch with the cool feeling function is slow, and the long-term cool feeling effect is excellent.
Experimental results show that the cool functional master batch provided by the preparation method has an instant cool coefficient of 0.17-0.25, an ultraviolet protection coefficient of 41-48, and excellent instant cool and ultraviolet resistance; the bacteriostatic rate of Candida albicans is 95%, the bacteriostatic rate of Staphylococcus aureus is 98%, the bacteriostatic rate of Escherichia coli is 96-99%, and the bacteriostatic rate is excellent.
Detailed Description
The invention provides a preparation method of a cool functional master batch, which comprises the following steps:
mixing the crystal jade with lithium nitrate, and carrying out hydrothermal ion exchange reaction to obtain nano-intercalation crystal jade;
mixing the nano-intercalation crystal jade, sulfuric acid, nitric acid and potassium permanganate, mixing the obtained mixture with zinc oxide, and modifying to obtain modified crystal jade;
and mixing the modified crystal jade, the resin carrier, the dispersing agent and the antioxidant, and performing melt blending and extrusion to obtain the cool functional master batch.
In the present invention, unless otherwise specified, commercially available products well known to those skilled in the art are used for each component in the preparation method.
The invention mixes the crystal jade with lithium nitrate to carry out hydrothermal ion exchange reaction, and obtains the nano intercalation crystal jade.
The invention is not particularly limited to the ice jade, and the ice jade known to those skilled in the art can be used. The source of the crystal jade is not particularly limited in the present invention, and any source known to those skilled in the art may be used. In the invention, the chemical composition of the ice jade comprises SiO2And trace elements including K, Ca, Al and Mg. In the present invention, the glacial jade belongs to the hexagonal system, and the Mohs hardness is 7 grade.
In the present invention, the particle size of the cryolite is preferably no greater than 500 nm. The present invention preferably grinds the cryolite before mixing it with the lithium nitrate. In the present invention, the grinding apparatus is preferably a pulverizer. In the present invention, the rotation speed in the grinding is preferably 3000 rpm; the invention does not specially limit the grinding, so as to ensure that the grain diameter of the crystal jade obtained by grinding is less than or equal to 500 nm.
In the invention, the mass ratio of the glacial jade to the lithium nitrate is preferably (80-95): (5-20), more preferably (85-92): (8-15), more preferably (91-92): (8-9).
In the invention, the temperature of the hydrothermal ion exchange reaction is preferably 150-180 ℃, and more preferably 155-175 ℃; the pressure is preferably 0.35 to 0.5MPa, more preferably 0.4 to 0.5 MPa. In the invention, the time of the hydrothermal ion exchange reaction is preferably 12-60 h, more preferably 24-48 h, and still more preferably 24-36 h.
In the invention, the particle size of the nano-intercalation crystal jade is preferably less than or equal to 100 nm.
In the invention, the glistening jade is mixed with lithium nitrate to carry out hydrothermal ion exchange reaction, lithium ions replace potassium ions between the glistening jade sheets, and simultaneously under the hydrothermal ion exchange reaction of a water phase, the lithium ions coat a hydration film, the hydration radius of the lithium ions is larger than that of the potassium ions, so that the aim of promoting the delamination of the silicon dioxide sheets of the glistening jade is fulfilled, the silicon dioxide powder of the glistening jade after the layered modification is further dispersed, the particle size is reduced, and the nano intercalation glistening jade with electric charge, high adsorption force, super-hydrophilicity, moisture absorption and cool effect is obtained.
After the nano intercalated crystal jade is obtained, the nano intercalated crystal jade, sulfuric acid, nitric acid and potassium permanganate are mixed, the obtained mixture is mixed with zinc oxide, and the mixture is modified to obtain the modified crystal jade.
In the present invention, the concentration of sulfuric acid is preferably 30% by mass. In the present invention, the concentration of nitric acid is preferably 10% by mass. In the invention, the mass ratio of the sulfuric acid to the nitric acid to the potassium permanganate is preferably (60-70): (10-20): (20) more preferably (60 to 65): (15-20): (15-20). In the invention, the mass ratio of the nano-intercalated icifuyu to the sulfuric acid is preferably (10-30): (70-90), more preferably (12-15): (85-88).
The invention mixes the nano intercalation crystal jade, sulfuric acid, nitric acid and potassium permanganate, which is beneficial to leading the nano intercalation crystal jade to generate-COOH functional groups.
In the present invention, the zinc oxide is preferably nano zinc oxide. In the present invention, the particle size of the zinc oxide is preferably 50 to 100 nm. In the present invention, the mass ratio of the zinc oxide to the mixed material (the mixed material is a mixture of the nano-intercalation crystal jade, sulfuric acid, nitric acid and potassium permanganate) is preferably 2: (98-100), more preferably 2: (99-100).
In the invention, the modification temperature is preferably 150-180 ℃, and more preferably 160-180 ℃; the time is preferably 3 to 6 hours, and more preferably 3 to 5 hours. According to the invention, modification can be carried out on the hexagonal crystal structure crystal jade through hydrothermal ion exchange reaction to obtain the lamellar structure nano intercalation crystal jade, so that the nano intercalation crystal jade has a larger surface area and is easy to crush to prepare nano particles with the particle size of 50-100 nm.
In the invention, the-COOH on the surface of the nano-intercalation crystal jade is combined with zinc ions generated by zinc oxide, thus being beneficial to forming a multi-layer and stable zinc ion-silicon dioxide grafting structure, improving the ultraviolet reflection performance of the modified crystal jade and being beneficial to obtaining the cool master batch with cool feeling and uvioresistant performance; and the zinc ions have excellent antibacterial performance, and are beneficial to obtaining the cool feeling functional master batch with antibacterial performance.
In the invention, the particle size of the modified crystal jade is preferably 100-200 nm, and more preferably 120-180 nm.
After the modified crystal jade is obtained, the modified crystal jade, the resin carrier, the dispersing agent and the antioxidant are mixed, and then are melted, blended and extruded to obtain the cool functional master batch.
In the present invention, the material of the resin carrier preferably includes one or more of polyethylene terephthalate (PET polyester), polybutylene terephthalate (PBT polyester) and polyamide 6(PA 6). In the present invention, the dispersant preferably includes one or more of polyethylene wax, ethylene bis stearamide, zinc stearate, polyethylene glycol 200, and polypropylene wax. In the present invention, the antioxidant preferably includes Trganox 1076 antioxidant and/or Trganox 168 antioxidant.
In the invention, the mass ratio of the modified crystal jade, the resin carrier, the dispersing agent and the antioxidant is preferably (68-78): (20-30): 1.5: 0.5, more preferably (68-75): (25-30): 1.5: 0.5.
in the present invention, the modified cryolite, the resin carrier, the dispersant and the antioxidant are preferably mixed by stirring. In the present invention, the stirring and mixing device is preferably a mixer. In the invention, the rotation speed of stirring and mixing is preferably 1200-1400 rpm, and more preferably 1250-1400 rpm; the time is preferably 12 to 15min, and more preferably 13 to 15 min.
In the present invention, the apparatus for melt blending extrusion is preferably a twin-screw extruder. In the invention, the temperature of the melt blending extrusion is preferably 260-290 ℃, and more preferably 265-285 ℃; the rotation speed of the screw is preferably 40 to 100rpm, more preferably 50 to 75 rpm.
In the present invention, after the melt blending extrusion, it is preferable to further include cooling and pelletizing in sequence. The present invention preferably cools the melt blended extruded product to room temperature. The pellets of the present invention are not particularly limited, and those known to those skilled in the art can be used. And cutting into granules to obtain the cool feeling functional master batch.
The invention also provides the cool feeling functional master batch prepared by the preparation method of the technical scheme.
The invention also provides cool fiber which comprises cool fiber filament and cool fiber short fiber, wherein the preparation material of the cool fiber comprises the cool functional master batch.
In the invention, the monofilament fineness of the cool fiber is preferably 0.8 to 3.33dtex, more preferably 0.9 to 3.1dtex, and still more preferably 1 to 3 dtex. The cross-sectional shape of the far infrared fiber is not particularly limited in the present invention, and the cross-sectional shape of the fiber known to those skilled in the art may be adopted, specifically, a circular shape, a triangular shape, a hollow shape or a flat shape.
The invention also provides a preparation method of the cool fiber in the technical scheme.
In the invention, when the cool fiber is a cool fiber filament, the preparation method of the cool fiber filament comprises the following steps:
mixing the cool functional master batch with the carrier slice, and spinning by a melting method to obtain pre-oriented yarn;
and (3) texturing the pre-oriented yarn to obtain the cool fiber filament.
The invention mixes the cool functional master batch with the carrier slice, and carries out melt spinning to obtain the pre-oriented yarn.
In the present invention, the cooling functional master batch is identical to the cooling functional master batch described in the above technical scheme, and is not described herein again.
In the present invention, when the cooling fiber is a cooling fiber filament, the carrier chip is preferably a polyethylene terephthalate chip and/or a polyamide chip.
In the present invention, when the cool fiber is a cool fiber filament, the mass ratio of the cool functional masterbatch to the carrier pellet is preferably 5: 95.
the melt spinning method of the present invention is not particularly limited, and the melt spinning method known to those skilled in the art may be used. In the present invention, when the cool fiber is a cool fiber filament, the melt spinning conditions include: the spinning temperature is preferably 260-282 ℃, and more preferably 265-280 ℃; the spinning speed is preferably 2000 to 3200m/min, more preferably 2200 to 3000 m/min.
After the pre-oriented yarn is obtained, the invention elasticizes the pre-oriented yarn to obtain the cool fiber filament.
The invention is not particularly limited to the texturing, and the texturing known to those skilled in the art may be adopted. In the invention, the elasticizing multiplying power of the elasticizing is preferably 1.5-1.6 times, and more preferably 1.5-1.55 times.
In the present invention, when the cool fiber is a cool fiber staple fiber, the method for preparing the cool fiber staple fiber comprises the steps of:
mixing the cool functional master batch with the carrier slice, carrying out melt spinning, and winding, molding and bundling the obtained fiber yarn to obtain raw yarn;
and sequentially carrying out subsequent drafting, shaping, curling and cutting on the protofilament to obtain the cool fiber staple fiber.
The invention mixes the cool functional master batch with the carrier slice, carries out melt spinning, and winds, shapes and bunches the obtained fiber yarn to obtain the protofilament.
In the present invention, the cooling functional master batch is identical to the cooling functional master batch described in the above technical scheme, and is not described herein again.
In the present invention, when the cooling fiber is a cooling fiber short fiber, the carrier chip is preferably a polyethylene terephthalate chip and/or a polyamide chip.
In the invention, when the cool fiber is cool fiber short fiber, the mass ratio of the cool functional master batch to the carrier slice is preferably (4-10): (90-96), more preferably (4-6): (94-96).
The melt spinning method of the present invention is not particularly limited, and the melt spinning method known to those skilled in the art may be used. In the present invention, when the cool fiber is a cool fiber staple fiber, the melt spinning conditions include: the spinning temperature is preferably 270-295 ℃, and more preferably 275-290 ℃; the spinning speed is preferably 900 to 1400m/min, more preferably 950 to 1100 m/min.
The winding, forming and bundling are not particularly limited in the present invention, and may be performed by winding, forming and bundling as well known to those skilled in the art.
After the precursor fiber is obtained, the precursor fiber is sequentially subjected to subsequent drafting, sizing, curling and cutting to obtain the cool fiber short fiber.
The drawing is not particularly limited in the present invention, and may be a drawing known to those skilled in the art. In the present invention, the draft ratio is preferably 3.0 to 4.5 times, and more preferably 3.2 to 4.3 times.
The present invention is not particularly limited to the setting, curling and cutting, and the setting, curling and cutting are well known to those skilled in the art.
The invention also provides application of the cool fiber in the technical scheme or the cool fiber prepared by the preparation method in the technical scheme in cool textiles.
The application of the invention is not particularly limited, and the application known to those skilled in the art can be adopted, and specifically, the cool feeling textile can be obtained by directly spinning the cool feeling fiber.
The present invention is not particularly limited to the above-mentioned textile, and may be one known to those skilled in the art.
In order to further illustrate the present invention, the following examples are provided to describe the cooling functional masterbatch, the cooling fiber, and the preparation method and application thereof in detail, but they should not be construed as limiting the scope of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The reagents used in the examples are all commercially available.
Example 1
Mixing 920g of crystal jade (the particle size is 50-100 nm) and 80g of lithium nitrate, and carrying out hydrothermal ion exchange reaction at 150 ℃ and 0.5MPa for 36h to obtain nano-intercalation crystal jade with the particle size less than or equal to 100 nm;
mixing 8000g of sulfuric acid (with the mass percentage concentration of 30%) and 2667g of nitric acid (with the mass percentage concentration of 10%) with 2667g of potassium permanganate, mixing the obtained mixture with 200g of zinc oxide (with the particle size of 50-100 nm), and modifying at 180 ℃ for 3 hours to obtain modified glimmer jade;
1500g of modified crystal jade, 3400g of resin carrier PET polyester chips, 75g of dispersant polypropylene wax and 5g of Trganox 168 antioxidant are placed in a mixer to be mixed with 1400rpm for 15min, then a double-screw extruder is used for carrying out melt blending extrusion under the conditions of 275 ℃ and 60rpm of screw rotation speed, and the mixture is cooled and cut into granules to obtain the cool functional master batch.
Example 2
5000g of the PET cool feeling functional master batch obtained in the example 1 and 95000g of PET polyester chips are mixed, and melt spinning is carried out under the conditions that the spinning temperature is 280 ℃ and the spinning speed is 2000m/min to obtain pre-oriented yarn;
and (3) texturing the pre-oriented yarn by a texturing multiple of 1.6 times to obtain the cool polyester DTY filament.
Example 3
5000g of PA6 polyamide cool feeling functional master batch obtained in example 1 and 95000gPA6 polyamide chips are mixed, melt spinning is carried out under the conditions that the spinning temperature is 270 ℃ and the spinning speed is 900m/min, and the obtained fiber yarn is wound, molded and bundled to obtain raw yarn;
and sequentially carrying out subsequent drafting, shaping, curling and cutting on the protofilament, wherein the drafting multiple is 3.2 times, and thus obtaining the cool fiber staple fiber.
The cool fibers obtained in the embodiments 2 to 3 are respectively prepared into cool fabrics and subjected to performance test, and the process for preparing the cool fabrics comprises the following steps: knitting plain cloth.
The performance test results of the cool fabric prepared from the cool fibers obtained in the examples 2-3 are shown in table 1.
Table 1 Performance test results of cool fabric prepared from cool fibers obtained in examples 2 to 3
As can be seen from Table 1, the cool fiber provided by the invention has an instant cool coefficient of 0.17-0.25, an ultraviolet protection coefficient of 41-48, and excellent instant cool and ultraviolet resistance; the bacteriostatic rate of Candida albicans is 95%, the bacteriostatic rate of Staphylococcus aureus is 98%, the bacteriostatic rate of Escherichia coli is 96-99%, and the bacteriostatic rate is excellent.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a cool functional master batch is characterized by comprising the following steps:
mixing the crystal jade with lithium nitrate, and carrying out hydrothermal ion exchange reaction to obtain nano-intercalation crystal jade;
mixing the nano-intercalation crystal jade, sulfuric acid, nitric acid and potassium permanganate, mixing the obtained mixture with zinc oxide, and modifying to obtain modified crystal jade;
and mixing the modified crystal jade, the resin carrier, the dispersing agent and the antioxidant, and performing melt blending and extrusion to obtain the cool functional master batch.
2. The method according to claim 1, wherein the hydrothermal ion exchange reaction is carried out at a temperature of 150 to 180 ℃ and a pressure of 0.35 to 0.5 MPa.
3. The preparation method according to claim 1, wherein the modification temperature is 150-180 ℃ and the modification time is 3-6 h.
4. The method according to claim 1, wherein the modified cryolite has a particle size of 100 to 200 nm.
5. A cool feeling functional masterbatch prepared by the preparation method of any one of claims 1 to 4.
6. A cool fiber comprising cool fiber filaments or cool fiber staple fibers, wherein the cool fiber comprises the cool functional masterbatch of claim 5.
7. The cooling fiber according to claim 6, wherein the monofilament fineness of the cooling fiber is 0.8 to 3.33 dtex.
8. The method for preparing a cool fiber according to claim 6 or 7, wherein when the cool fiber is a cool fiber filament, the method for preparing the cool fiber filament comprises the steps of:
mixing the cool functional master batch with the carrier slice, and spinning by a melting method to obtain pre-oriented yarn;
and (3) texturing the pre-oriented yarn to obtain the cool fiber filament.
9. The method for producing a cooling fiber according to claim 6 or 7, wherein when the cooling fiber is a cooling fiber staple, the method for producing a cooling fiber staple comprises the steps of:
mixing the cool functional master batch with the carrier slice, carrying out melt spinning, and winding, molding and bundling the obtained fiber yarn to obtain raw yarn;
and sequentially carrying out subsequent drafting, shaping, curling and cutting on the protofilament to obtain the cool fiber staple fiber.
10. Use of the cool fiber according to any one of claims 6 to 7 or the cool fiber prepared by the preparation method according to any one of claims 8 to 9 in cool textiles.
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| CN116411359A (en) * | 2023-04-19 | 2023-07-11 | 桐昆集团股份有限公司 | Production method and equipment of cool-feeling antibacterial fiber |
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| CN201473628U (en) * | 2009-07-28 | 2010-05-19 | 凯翔科技有限公司 | Mica yarn |
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| CN201473628U (en) * | 2009-07-28 | 2010-05-19 | 凯翔科技有限公司 | Mica yarn |
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| CN116411359A (en) * | 2023-04-19 | 2023-07-11 | 桐昆集团股份有限公司 | Production method and equipment of cool-feeling antibacterial fiber |
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