CN113584626A - Intelligent temperature control type meta-aramid fiber and preparation method thereof - Google Patents
Intelligent temperature control type meta-aramid fiber and preparation method thereof Download PDFInfo
- Publication number
- CN113584626A CN113584626A CN202110732870.8A CN202110732870A CN113584626A CN 113584626 A CN113584626 A CN 113584626A CN 202110732870 A CN202110732870 A CN 202110732870A CN 113584626 A CN113584626 A CN 113584626A
- Authority
- CN
- China
- Prior art keywords
- paraffin
- meta
- stirring
- solution
- preparing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920006231 aramid fiber Polymers 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 179
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 179
- 239000012188 paraffin wax Substances 0.000 claims abstract description 158
- 239000003094 microcapsule Substances 0.000 claims abstract description 154
- 239000002131 composite material Substances 0.000 claims abstract description 110
- 238000009987 spinning Methods 0.000 claims abstract description 48
- 238000002166 wet spinning Methods 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 22
- 230000008859 change Effects 0.000 claims abstract description 17
- 239000011162 core material Substances 0.000 claims abstract description 11
- 229920002635 polyurethane Polymers 0.000 claims abstract description 5
- 239000004814 polyurethane Substances 0.000 claims abstract description 5
- WRDNCFQZLUCIRH-UHFFFAOYSA-N 4-(7-azabicyclo[2.2.1]hepta-1,3,5-triene-7-carbonyl)benzamide Chemical compound C1=CC(C(=O)N)=CC=C1C(=O)N1C2=CC=C1C=C2 WRDNCFQZLUCIRH-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229920000162 poly(ureaurethane) Polymers 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 193
- 238000003756 stirring Methods 0.000 claims description 168
- 238000002156 mixing Methods 0.000 claims description 105
- 239000012074 organic phase Substances 0.000 claims description 100
- 239000008346 aqueous phase Substances 0.000 claims description 76
- 238000005406 washing Methods 0.000 claims description 70
- 238000001035 drying Methods 0.000 claims description 66
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 65
- 238000004945 emulsification Methods 0.000 claims description 63
- LXEJRKJRKIFVNY-UHFFFAOYSA-N terephthaloyl chloride Chemical compound ClC(=O)C1=CC=C(C(Cl)=O)C=C1 LXEJRKJRKIFVNY-UHFFFAOYSA-N 0.000 claims description 63
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 60
- 239000004760 aramid Substances 0.000 claims description 56
- 229920003235 aromatic polyamide Polymers 0.000 claims description 56
- 239000012071 phase Substances 0.000 claims description 37
- 238000010438 heat treatment Methods 0.000 claims description 34
- 239000008367 deionised water Substances 0.000 claims description 33
- 229910021641 deionized water Inorganic materials 0.000 claims description 33
- 239000000839 emulsion Substances 0.000 claims description 32
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 30
- 239000006185 dispersion Substances 0.000 claims description 22
- 230000010355 oscillation Effects 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000003995 emulsifying agent Substances 0.000 claims description 9
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 8
- -1 polyoxyethylene octylphenol Polymers 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 6
- 230000001804 emulsifying effect Effects 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 238000009775 high-speed stirring Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 125000001140 1,4-phenylene group Chemical group [H]C1=C([H])C([*:2])=C([H])C([H])=C1[*:1] 0.000 claims description 4
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 4
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 4
- 239000011550 stock solution Substances 0.000 claims description 4
- 238000012695 Interfacial polymerization Methods 0.000 claims description 3
- 229920001214 Polysorbate 60 Polymers 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 3
- 239000000194 fatty acid Substances 0.000 claims description 3
- 229930195729 fatty acid Natural products 0.000 claims description 3
- 150000002191 fatty alcohols Chemical class 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- KVNYFPKFSJIPBJ-UHFFFAOYSA-N ortho-diethylbenzene Natural products CCC1=CC=CC=C1CC KVNYFPKFSJIPBJ-UHFFFAOYSA-N 0.000 claims description 2
- 150000005215 alkyl ethers Chemical class 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 24
- 239000012782 phase change material Substances 0.000 abstract description 18
- 230000008569 process Effects 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 62
- CBFCDTFDPHXCNY-UHFFFAOYSA-N icosane Chemical compound CCCCCCCCCCCCCCCCCCCC CBFCDTFDPHXCNY-UHFFFAOYSA-N 0.000 description 36
- 238000009998 heat setting Methods 0.000 description 32
- 238000009740 moulding (composite fabrication) Methods 0.000 description 32
- 238000002844 melting Methods 0.000 description 31
- 230000008018 melting Effects 0.000 description 31
- 230000008023 solidification Effects 0.000 description 29
- 238000007711 solidification Methods 0.000 description 29
- 229960001701 chloroform Drugs 0.000 description 27
- 239000011575 calcium Substances 0.000 description 25
- RZJRJXONCZWCBN-UHFFFAOYSA-N octadecane Chemical compound CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 description 22
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 18
- VAMFXQBUQXONLZ-UHFFFAOYSA-N n-alpha-eicosene Natural products CCCCCCCCCCCCCCCCCCC=C VAMFXQBUQXONLZ-UHFFFAOYSA-N 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 10
- 239000004744 fabric Substances 0.000 description 9
- 239000004753 textile Substances 0.000 description 7
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229920000136 polysorbate Polymers 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- BJQWYEJQWHSSCJ-UHFFFAOYSA-N heptacosane Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCC BJQWYEJQWHSSCJ-UHFFFAOYSA-N 0.000 description 2
- 239000012510 hollow fiber Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 229920003366 poly(p-phenylene terephthalamide) Polymers 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004970 Chain extender Substances 0.000 description 1
- 206010063385 Intellectualisation Diseases 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229920002396 Polyurea Polymers 0.000 description 1
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002457 bidirectional effect Effects 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012975 dibutyltin dilaurate Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 239000013074 reference sample Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
Images
Classifications
-
- 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
- D01F6/905—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 of aromatic polyamides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
- B01J13/16—Interfacial polymerisation
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Carbon And Carbon Compounds (AREA)
- Inorganic Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses an intelligent temperature control type meta-aramid fiber and a preparation method thereof, wherein a phase change microcapsule is added into a meta-aramid fiber spinning solution, and spinning is completed by adopting wet spinning, so that the intelligent temperature control type meta-aramid fiber is obtained, the phase change microcapsule comprises a wall material and a core material wrapped in the wall material, the wall material adopts poly-p-phenylene terephthalamide, polyurea or polyurethane, the core material adopts a paraffin/graphene composite material, the paraffin/graphene composite material accounts for 20-75% of the mass of the phase change microcapsule, and the phase change microcapsule accounts for 3-20% of the mass of the intelligent temperature control type meta-aramid fiber. The invention has simple process, good temperature control effect, low cost of the selected phase-change material and difficult loss of the phase-change material in the fiber.
Description
Technical Field
The invention belongs to the technical field of meta-aramid, and particularly relates to intelligent temperature control meta-aramid and a preparation method thereof.
Background
The meta-aramid fiber is a high-performance special fiber, has excellent performances of flame retardance, high temperature resistance, electric insulation, high strength, chemical corrosion resistance and the like, and is mainly applied to the fields of individual protection and industry. The demands of personal protection in the new period place higher demands on protective materials, protective garments and protective technology, such as functional integration. The ability of the fibers to control temperature during ambient temperature changes provides the wearer with a relatively comfortable and safe in-garment microenvironment in extreme environments. The temperature control fiber is mainly used for astronaut clothing and jackets of some precision instruments in the initial research, and the intelligent temperature control meta-aramid fiber is produced along with the increasing demand for high-quality and high-performance textiles.
The temperature control capability of the fiber is generally realized by adding phase change materials into the fiber, and the fiber has a bidirectional regulation function. When the temperature of the external environment rises, the phase change material contained in the fiber is changed into liquid from solid, absorbs heat and stores the heat in the fiber; when the external environment temperature is reduced, the phase-change material is changed from a liquid state to a solid state, the stored heat is released, the body sensing temperature is kept in a small range, and a human body is in a comfortable state. The heat absorption and release process of the intelligent temperature control fiber is automatic, reversible and infinite.
Since the world, the phase change material has attracted much attention of researchers due to its intellectualization and autonomy, and is now widely used in intelligent products such as buildings, solar energy, and home appliances, and in the textile field, the phase change material is relatively still under further study and development.
The preparation method for combining the phase-change material and the chemical fiber mainly comprises the following steps: blending method, micro-encapsulation method, hollow fiber filling method and post-finishing method. Patent No. CN104153203A relates to an intelligent temperature-regulating textile and a preparation method thereof, wherein a coating adhesive is adopted to coat and mix phase-change microcapsules, and then the phase-change microcapsules are coated on the surface of a textile fabric to prepare the intelligent temperature-regulating textile. The method belongs to the field of after finishing, the after finishing method is simple and easy to operate, but the fabric is easy to fall off in the using and washing and protecting processes, and the durability of the functional effect needs to be further improved; the hollow fiber filling method is relatively complicated to operate; the blending method has the problems that the phase-change material is easy to run off and the like; the microcapsule technology successfully wraps the phase-change material in a specific wall material, and effectively solves the problem of leakage in practical application.
Disclosure of Invention
The invention aims to provide an intelligent temperature control type meta-aramid fiber and a preparation method thereof, which overcome the defects of the prior art, and have the advantages of simple process, good temperature control effect, low cost of the selected phase-change material and difficult loss of the phase-change material in the fiber.
In order to achieve the purpose, the invention adopts the following technical scheme:
the method for preparing the intelligent temperature control type meta-aramid comprises the steps of adding phase change microcapsules into meta-aramid spinning stock solution, and completing spinning by adopting wet spinning to obtain the intelligent temperature control type meta-aramid, wherein the phase change microcapsules comprise a wall material and a core material wrapped in the wall material, the wall material adopts poly-p-phenylene terephthalamide, polyurea or polyurethane, the core material adopts a paraffin/graphene composite material, the paraffin/graphene composite material accounts for 20-75% of the mass of the phase change microcapsules, and the phase change microcapsules account for 3-20% of the mass of the intelligent temperature control type meta-aramid.
Further, in the paraffin/graphene composite material, paraffin adopts straight-chain paraffin, and the molecular formula of the paraffin/graphene composite material is CxH2x+2X is more than or equal to 16 and less than or equal to 27; when the wall material adopts poly-p-phenylene terephthamide, the molecular structure is
40≤n≤200。
Further, the phase-change microcapsule is prepared by adopting an interfacial polymerization method, and the method comprises the following specific steps:
(1) adding an emulsifier into deionized water, stirring and mixing uniformly to form an emulsified solution, and then adding an acid-binding agent to obtain a water phase;
(2) adding a paraffin/graphene composite material and terephthaloyl chloride into an organic solvent, and uniformly stirring and mixing to obtain an organic phase;
(3) and dispersing the uniformly mixed organic phase in a water phase under high-speed stirring, emulsifying, adjusting the stirring speed after the emulsification is finished, adding the prepared p-phenylenediamine solution into the emulsion, finishing the reaction when the pH value of the system is not changed, filtering, washing and drying to obtain the phase-change microcapsule.
Further, the preparation process of the paraffin/graphene composite material is as follows: heating paraffin at 75 ℃ until the paraffin is completely in a uniform liquid state, adding graphene into the paraffin, stirring for 30-100 min, and then performing ultrasonic oscillation dispersion to obtain a paraffin/graphene composite material; wherein the mass fraction of graphene in the paraffin/graphene composite material is 1-10%.
Further, the emulsifier in the step (1) is one or two of polyoxyethylene octyl phenol ether-10, fatty alcohol polyoxyethylene ether C12 and polyoxyethylene sorbitan fatty acid ester, and each 100mL of the emulsifying solution contains 5-25 mL of the emulsifier.
Further, in the step (1), the acid-binding agent is one of sodium hydroxide, calcium hydroxide and sodium bicarbonate; the organic solvent in the step (2) is one of chloroform, diethyl ether, benzene and toluene.
Further, the stirring and mixing time in the step (1) is 15-60 min, and the stirring and mixing time in the step (2) is 30-80 min; and (4) in the step (3), the high-speed stirring speed is 3000-8000 rpm, and the stirring speed is adjusted to be 400-800 rpm after emulsification is finished.
Furthermore, the mass ratio of the organic phase to the water phase is (85-98): 2-15).
Furthermore, the molar ratio of the terephthaloyl chloride to the p-phenylenediamine is 1 (1.1-2.2), and the mass concentration of the p-phenylenediamine solution in the step (3) is 5-20%.
The intelligent temperature control type meta-aramid fiber is prepared by the preparation method of the intelligent temperature control type meta-aramid fiber.
Compared with the prior art, the invention has the following beneficial technical effects:
in the existing research and application, microencapsulation is adopted and then the fiber or the fabric is coated with a post-finishing coating, or the fiber or the fabric is prepared by spinning after being blended with a spinning stock solution, but the microcapsule is directly added into the spinning stock solution, so that the problem of loss of a phase-change material due to microcapsule breakage easily occurs. The invention selects the wall material poly-p-phenylene terephthamide, the prepared microcapsule has higher coating rate to the phase-change material, and the poly-p-phenylene terephthamide has excellent high temperature resistance, can well protect the core material phase-change material from being lost easily in the spinning drying heat treatment process, and still has higher temperature control capability after being washed for many times.
The method comprises the steps of adding phase-change microcapsules into a spinning solution for preparing the meta-aramid through wet spinning, and then carrying out spinning forming, washing, drying, heat setting and the like to obtain the intelligent temperature-control meta-aramid. The phase-change microcapsule core material is paraffin with stable performance, no toxicity, no corrosiveness, low cost, higher phase-change latent heat and high crystallization rate, the wall material is a high-temperature-resistant polymer, and the graphene is added in the process of preparing the microcapsule to increase the heat conduction performance of the paraffin.
Drawings
The accompanying drawings are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a graph showing the surface temperature of the fiber sample textile fabrics of example 7, comparative example 1 and comparative example 2 as a function of ambient temperature;
FIG. 3 is the surface temperature of the fabric of example 7 after washing with water for 50 times as a function of the ambient temperature;
FIG. 4 is a schematic cross-sectional view of a smart temperature control fiber;
FIG. 5 is a CV control diagram of the coagulation bath concentration during spinning;
FIG. 6 is a CV control diagram of the water wash flow during spinning.
Detailed Description
The invention is described in further detail below:
referring to fig. 1, a method for preparing intelligent temperature-control meta-aramid adopts wet spinning, a certain amount of phase-change microcapsules are added into a spinning solution, then processes of spinning forming, washing, drying, heat setting and the like are carried out, so that the intelligent temperature-control meta-aramid (as shown in fig. 4) is obtained, the mass fraction of the phase-change microcapsules in the intelligent temperature-control meta-aramid is 3% -20%, and when the environmental temperature of the prepared intelligent temperature-control meta-aramid changes, the temperature of the surface of the fiber can be automatically adjusted, the body surface is maintained at a comfortable temperature, and the comfort of the meta-aramid in the field of individual protection is improved.
The phase-change microcapsule takes a paraffin/graphene composite material as a core material, one of poly-p-phenylene terephthalamide (PPTA), polyurea and polyurethane as a wall material, and the core material is wrapped by the wall material to prepare the phase-change microcapsule.
The paraffin in the core material is straight-chain paraffin, and the molecular formula of the paraffin is CxH2x+2X is more than or equal to 16 and less than or equal to 27, the wall material takes PPTA as an example, and the molecular structure is
N is more than or equal to 40 and less than or equal to 200, and the phase-change microcapsule is prepared by adopting an interfacial polymerization method, and the specific steps are as follows:
(1) preparing a water phase: adding a proper amount of emulsifier into deionized water, stirring and mixing uniformly to form an emulsified solution, and then adding a certain amount of acid-binding agent; the emulsifier is one or two of polyoxyethylene octyl phenol ether-10 (OP-10), fatty alcohol polyoxyethylene volumetric ether C12(AEO-3), polyoxyethylene sorbitan fatty acid ester (Tween) series and the like, the dosage of the emulsifier is 5-25 ml/100ml of emulsified solution, the stirring and mixing time is 15-60 min, and the acid-binding agent is one of sodium hydroxide, calcium hydroxide, sodium bicarbonate and the like;
(2) preparing an organic phase: adding a proper amount of paraffin/graphene composite material and terephthaloyl chloride (TPC) into an organic solvent, and stirring and mixing for 30-80 min; the dosage of the paraffin/graphene composite material is 20-75% of the mass of the phase-change microcapsule, and the mass fraction of graphene in the paraffin/graphene composite material is 1-10%; the organic solvent in the organic phase preparation is one of trichloromethane, diethyl ether, benzene, toluene and the like;
the preparation method of the paraffin/graphene composite material comprises the following steps: heating paraffin at 75 ℃, slowly adding graphene into the paraffin, stirring for a certain time, and then ultrasonically oscillating and dispersing to obtain the paraffin/graphene composite material, wherein the composite material containing different graphene contents can be prepared according to requirements.
(3) The preparation process of the microcapsule comprises the following steps: firstly, dispersing an organic phase after uniform mixing in a water phase under high-speed stirring at 3000-8000 rpm, carrying out emulsification treatment, wherein the mass ratio of the organic phase to the water phase is (85-98): (2-15), after emulsification is finished, adjusting the stirring speed to 400-800 rpm, adding a prepared p-Phenylenediamine (PDA) solution with the mass concentration of 5-20% into an emulsion, wherein the molar ratio of terephthaloyl chloride to p-phenylenediamine is 1 (1.1-2.2), when the pH value of a system is not changed, finishing the reaction, and then filtering, washing (adopting ethanol) and drying.
The present invention will be described in detail with reference to examples. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The following detailed description is illustrative of the embodiments and is intended to provide further details of the invention. Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention.
Example 1
Preparing a paraffin/graphene composite material: heating and melting n-octadecane at 75 ℃, slowly adding graphene into the melted paraffin, wherein the content of the graphene is 2%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 20% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 2
Preparing a paraffin/graphene composite material: heating and melting n-eicosane at 75 ℃, slowly adding graphene into the melted paraffin, stirring for a certain time, and then ultrasonically oscillating and dispersing to obtain the paraffin/graphene composite material, wherein the content of the graphene is 2%.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 20% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 3
Preparing a paraffin/graphene composite material: heating and melting the n-hexadecane and n-eicosane in a ratio of 1:1 at 75 ℃, slowly adding graphene into the melted paraffin with the graphene content being 2%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 20% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 4
Preparing a paraffin/graphene composite material: heating and melting n-octadecane at 75 ℃, slowly adding graphene into the melted paraffin, wherein the content of the graphene is 5%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 20% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, stirring and mixingUniformly mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 5
Preparing a paraffin/graphene composite material: heating and melting n-eicosane at 75 ℃, slowly adding graphene into the melted paraffin, stirring for a certain time, and then ultrasonically oscillating and dispersing to obtain the paraffin/graphene composite material, wherein the content of the graphene is 5%.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 20% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 6
Preparing a paraffin/graphene composite material: heating and melting the n-hexadecane and n-eicosane in a ratio of 1:1 at 75 ℃, slowly adding graphene into the melted paraffin with the graphene content being 5%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 20% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 7
Preparing a paraffin/graphene composite material: heating and melting n-octadecane at 75 ℃, slowly adding graphene into the melted paraffin, wherein the content of the graphene is 8%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 20% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; then, under the condition of stirring speed of 3000rpm, pouring organic phase solution into water phase, making the mass ratio of organic phase and water phase be 95:5, making emulsification treatment, regulating stirring speed to 400rpm, then mixing the above-mentioned materials to obtain the invented product with 15% mass concentrationAdding the PDA solution into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, finishing the reaction, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 8
Preparing a paraffin/graphene composite material: heating and melting n-eicosane at 75 ℃, slowly adding graphene into the melted paraffin, stirring for a certain time, and then ultrasonically oscillating and dispersing to obtain the paraffin/graphene composite material, wherein the content of the graphene is 8%.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 20% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 9
Preparing a paraffin/graphene composite material: heating and melting the n-hexadecane and n-eicosane in a ratio of 1:1 at 75 ℃, slowly adding graphene into the melted paraffin with the graphene content being 8%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 20% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 10
Preparing a paraffin/graphene composite material: heating and melting n-octadecane at 75 ℃, slowly adding graphene into the melted paraffin, wherein the content of the graphene is 5%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 25% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 11
Preparing a paraffin/graphene composite material: heating and melting n-eicosane at 75 ℃, slowly adding graphene into the melted paraffin, stirring for a certain time, and then ultrasonically oscillating and dispersing to obtain the paraffin/graphene composite material, wherein the content of the graphene is 5%.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 25% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 12
Preparing a paraffin/graphene composite material: heating and melting the n-hexadecane and n-eicosane in a ratio of 1:1 at 75 ℃, slowly adding graphene into the melted paraffin with the graphene content being 5%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 25% paraffin/graphene into trichloromethaneUniformly stirring and mixing the composite material and 20.303g of TPC to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 13
Preparing a paraffin/graphene composite material: heating and melting n-octadecane at 75 ℃, slowly adding graphene into the melted paraffin, wherein the content of the graphene is 5%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 30% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 14
Preparing a paraffin/graphene composite material: heating and melting n-eicosane at 75 ℃, slowly adding graphene into the melted paraffin, stirring for a certain time, and then ultrasonically oscillating and dispersing to obtain the paraffin/graphene composite material, wherein the content of the graphene is 5%.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 30% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 15
Preparing a paraffin/graphene composite material: heating and melting the n-hexadecane and n-eicosane in a ratio of 1:1 at 75 ℃, slowly adding graphene into the melted paraffin with the graphene content being 5%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 30% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; then, under the condition of stirring speed of 3000rpm, pouring organic phase solution into water phase, making the mass ratio of organic phase to water phase be 95:5, making emulsification treatment so as to implement emulsification, regulating stirring speedAt 400rpm, adding a 15% PDA solution into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, the reaction is finished, washing the microcapsule with ethanol, and drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 16
Preparing a paraffin/graphene composite material: heating and melting n-heptacosane at 75 ℃, slowly adding graphene into the melted paraffin, wherein the content of the graphene is 1%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding 8ml/100ml of OP-10 into deionized water, stirring and mixing uniformly, and then adding 4g of sodium hydroxide to prepare an aqueous phase solution; (2) adding 25% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 5% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.3, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 17
Preparing a paraffin/graphene composite material: heating and melting n-eicosane at 75 ℃, slowly adding graphene into the melted paraffin, stirring for a certain time, and then ultrasonically oscillating and dispersing to obtain the paraffin/graphene composite material, wherein the content of the graphene is 3%.
Preparing microcapsules: (1) adding 10ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 25% of paraffin/graphene composite material and 20.303g of TPC into diethyl ether, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 16% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.3, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 18
Preparing a paraffin/graphene composite material: heating and melting the n-hexadecane and n-eicosane in a ratio of 1:1 at 75 ℃, slowly adding graphene into the melted paraffin with the graphene content being 6%, stirring for a certain time, and then performing ultrasonic oscillation and dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding 15ml/100ml of OP-10 into deionized water, stirring and mixing uniformly, and then adding 8.4g of sodium bicarbonate to prepare an aqueous phase solution; (2) adding 25% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then pouring the organic phase solution into the water phase at a stirring speed of 7000rpm, carrying out emulsification treatment when the mass ratio of the organic phase to the water phase is 95:5, completing emulsification, adjusting the stirring speed to 400rpm, then adding the PDA solution with the prepared mass concentration of 16% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.3, when the pH value of the system is not changed, washing the microcapsule with ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 5%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 19
Preparing a paraffin/graphene composite material: heating and melting n-octadecane at 75 ℃, slowly adding graphene into the melted paraffin, wherein the content of the graphene is 8%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding AEO-3 20ml/100ml into deionized water, stirring, mixing, adding Ca (OH) 7.4g2Preparing an aqueous phase solution; (2) adding 25% of paraffin/graphene composite material and 20.303g of TPC into benzene, stirring and mixing uniformly to prepare an organic phase solution; and then, under the condition that the stirring speed is 6000rpm, pouring an organic phase solution into an aqueous phase, carrying out emulsification treatment according to the mass ratio of the organic phase to the aqueous phase of 95:5, finishing emulsification, adjusting the stirring speed to 400rpm, adding a PDA solution with the well-prepared mass concentration of 18.5% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.5, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution to obtain a blended solution, and then carrying out wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature-control meta-aramid.
Example 20
Preparing a paraffin/graphene composite material: heating and melting n-eicosane at 75 ℃, slowly adding graphene into the melted paraffin, stirring for a certain time, and then ultrasonically oscillating and dispersing to obtain the paraffin/graphene composite material, wherein the content of the graphene is 10%.
Preparing microcapsules: (1) adding 5ml/100ml Tween into deionized water, stirring, mixing, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 25% paraffin/graphene into trichloromethaneMixing the materials with 20.303g of TPC, stirring and mixing uniformly to prepare an organic phase solution; and then, under the condition that the stirring speed is 5000rpm, pouring an organic phase solution into an aqueous phase, carrying out emulsification treatment when the mass ratio of the organic phase to the aqueous phase is 95:5, finishing emulsification, adjusting the stirring speed to 800rpm, then adding a PDA solution with the well-prepared mass concentration of 18.5% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.5, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 8%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 21
Preparing a paraffin/graphene composite material: heating and melting the n-hexadecane and n-eicosane in a ratio of 1:1 at 75 ℃, slowly adding graphene into the melted paraffin with the graphene content being 5%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding 5ml/100ml Tween into deionized water, stirring, mixing, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 60% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 4000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 18.5% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.5, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 22
Preparing a paraffin/graphene composite material: heating and melting n-octadecane at 75 ℃, slowly adding graphene into the melted paraffin, wherein the content of the graphene is 5%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding 25ml/100ml of OP-10 into deionized water, stirring and mixing uniformly, and then adding 4g of sodium hydroxide to prepare an aqueous phase solution; (2) adding 50% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution to obtain a blended solution, and then carrying out wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature-control meta-aramid.
Example 23
Preparing a paraffin/graphene composite material: heating and melting n-eicosane at 75 ℃, slowly adding graphene into the melted paraffin, stirring for a certain time, and then ultrasonically oscillating and dispersing to obtain the paraffin/graphene composite material, wherein the content of the graphene is 5%.
Preparing microcapsules: (1) adding 5ml/100ml AEO-3 into deionized water, stirring and mixing well, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 25% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; then, under the condition of stirring speed of 3000rpm, pouring organic phase solution into water phase, making organic phase and water phase be mixed according to the mass ratio of 93:7, making emulsification treatment so as to obtain the invented product with 4 stirring speedAnd (3) 00rpm, adding a 20% PDA solution with the prepared mass concentration into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, finishing the reaction, washing the microcapsule by using ethanol, and drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution to obtain a blended solution, and then carrying out wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature-control meta-aramid.
Example 24
Preparing a paraffin/graphene composite material: heating and melting the n-hexadecane and n-eicosane in a ratio of 1:1 at 75 ℃, slowly adding graphene into the melted paraffin with the graphene content being 5%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding 5ml/100ml of OP-10 into deionized water, stirring and mixing uniformly, and then adding 10.6g of sodium carbonate to prepare an aqueous phase solution; (2) adding 40% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution to obtain a blended solution, and then carrying out wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature-control meta-aramid.
Example 25
Preparing a paraffin/graphene composite material: heating and melting n-octadecane at 75 ℃, slowly adding graphene into the melted paraffin, wherein the content of the graphene is 5%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 20% of paraffin/graphene composite material and 20.303g of TPC into toluene, stirring and mixing uniformly to prepare an organic phase solution; and then, pouring the organic phase solution into the water phase at a stirring speed of 8000rpm, wherein the mass ratio of the organic phase to the water phase is 90:10, emulsifying to complete emulsification, adjusting the stirring speed to 500rpm, adding the PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution to obtain a blended solution, and then carrying out wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature-control meta-aramid.
Example 26
Preparing a paraffin/graphene composite material: heating and melting n-eicosane at 75 ℃, slowly adding graphene into the melted paraffin, stirring for a certain time, and then ultrasonically oscillating and dispersing to obtain the paraffin/graphene composite material, wherein the content of the graphene is 5%.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 25% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 600rpm, then adding a PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution to obtain a blended solution, and then carrying out wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature-control meta-aramid.
Example 27
Preparing a paraffin/graphene composite material: heating and melting the n-hexadecane and n-eicosane in a ratio of 1:1 at 75 ℃, slowly adding graphene into the melted paraffin with the graphene content being 5%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 75% of paraffin/graphene composite material and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 90:10, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 700rpm, then adding a PDA solution with the well-prepared mass concentration of 5% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 15%, preparing the blended solution, then performing wet spinning, coagulating and forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 28
Preparing a paraffin/graphene composite material: heating and melting n-octadecane at 75 ℃, slowly adding graphene into the melted paraffin, wherein the content of the graphene is 8%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
The wall material is polyurea, and the microcapsule is prepared as follows: (1) adding OP-10 of 8ml/100ml into deionized water, stirring and mixing uniformly, adding 7.4g of Ca (OH)2Preparation of aqueous phaseLiquid; (2) adding 20% of paraffin/graphene composite material and 17.416g of 2, 4-Toluene Diisocyanate (TDI) into trichloromethane, and stirring and mixing uniformly to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring the organic phase solution into the water phase, wherein the mass ratio of the organic phase system to the water phase system is 90:10, carrying out emulsification treatment to complete emulsification, the stirring speed is adjusted to 700rpm, then adding an Ethylene Diamine (EDA) solution with the prepared mass concentration of 20% into the emulsion, wherein the molar ratio of TDI to EDA is 1:1.2, when the pH value of the system is not changed, finishing the reaction, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Example 29
Preparing a paraffin/graphene composite material: heating and melting n-octadecane at 75 ℃, slowly adding graphene into the melted paraffin, wherein the content of the graphene is 8%, stirring for a certain time, and then performing ultrasonic oscillation dispersion to obtain the paraffin/graphene composite material.
The wall material is polyurethane, and the microcapsule is prepared by the following steps: (1) adding 8ml/100ml of OP-10 into deionized water, and uniformly stirring and mixing to prepare an aqueous phase solution; (2) adding 20% of paraffin/graphene composite material, 17.416g of 2, 4-Toluene Diisocyanate (TDI) and dibutyltin dilaurate with the mass concentration of 1% of an oil phase system into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring the organic phase solution into the water phase, wherein the mass ratio of the organic phase system to the water phase system is 90:10, carrying out emulsification treatment, completing emulsification, adjusting the stirring speed to 400rpm, adding 18g of polyethylene glycol (PEG: molecular weight 800), carrying out prepolymerization reaction for 30min, then heating to 40 ℃, adding 5g of chain extender glycol, continuing to react for 40min, after the reaction is finished, washing the microcapsule with ethanol, and then drying.
Preparing meta-aramid: and (2) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 3%, preparing the blended solution, and then performing wet spinning, solidification forming, washing, drying, heat setting and the like to obtain the intelligent temperature control meta-aramid fiber.
Comparative example 1
Preparing microcapsules: (1) adding 5ml/100ml OP-10 into deionized water, stirring and mixing uniformly, adding 7.4g Ca (OH)2Preparing an aqueous phase solution; (2) adding 25% of paraffin (n-octadecane) and 20.303g of TPC into trichloromethane, and uniformly stirring and mixing to prepare an organic phase solution; and then, under the condition that the stirring speed is 3000rpm, pouring an organic phase solution into an aqueous phase, wherein the mass ratio of the organic phase to the aqueous phase is 95:5, carrying out emulsification treatment to complete emulsification, adjusting the stirring speed to 400rpm, then adding a PDA solution with the well-prepared mass concentration of 15% into the emulsion, wherein the molar ratio of TPC to PDA is 1:1.2, when the pH value of the system is not changed, washing the microcapsule by using ethanol, and then drying.
Preparing meta-aramid: and (3) blending the microcapsules and the spinning solution, wherein the content of the microcapsules in the meta-aramid fiber is 20%, preparing the blended solution, then performing wet spinning, performing solidification forming, washing, drying, heat setting and the like to obtain the reference sample 1-meta-aramid fiber.
Comparative example 2
And taking the conventional meta-aramid as a comparison sample of 2-meta-aramid.
The properties of the phase change microcapsules and fibers prepared in the examples and comparative examples are shown in table 1:
TABLE 1 Performance index for the preparation of microcapsules and of meta-aramid
Through the performance detection of the microcapsule and the fiber, the result shows that the heat conductivity of the microcapsule is obviously improved by adding the graphene, particularly, the heat conductivity of the embodiment 7 is increased to 2.01W/m.K, and is improved by 9 times compared with the heat conductivity of the comparative ratio 1 of 0.22. The mechanical property of the meta-aramid fiber obtained by adding the phase-change microcapsule is reduced, but the meta-aramid fiber still keeps high breaking strength and elongation at break. The LOI values of the detected fiber samples are all above 30%, and compared with the conventional meta-aramid fiber, the LOI of the phase-change microcapsule is slightly reduced, but the good flame retardance is still maintained.
The fiber samples of example 7, comparative example 1 and comparative example 2 were selected for textile fabric, and the temperature control conditions of the intelligent temperature control fibers after multiple water washes were tested.
The temperature change curve is drawn by monitoring the surface temperature of the fabric in the embodiment 7, the comparative example 1 and the comparative example 2, as shown in fig. 2, when the temperature does not reach the melting point, the temperature rise speed is high, after the temperature reaches the melting point, the phase change material absorbs the external heat to be stored in a latent heat mode and starts to melt, and after the phase change is completed, the temperature rise speed is increased again. The cooling phase is similar with the phase process that heaies up, and when the temperature did not reach phase change material's freezing point, the temperature is fast relatively that reduces, and when reaching the freezing point, phase change material released its latent heat of storing, can maintain fibre surface temperature in the phase change temperature scope, formed one section temperature platform, waits to solidify the back cooling rate of cooling once more completely. And comparing whether the microcapsule of the graphene is added or not, and finding that the graphene can improve the heat conduction capability of the paraffin.
The temperature control monitoring comparison is carried out on the fabric of example 7 before and after 50 times of water washing, and as shown in fig. 3, the phase change microcapsules have good stability in the fibers and still have good temperature control capability.
Fig. 5 and 6 are control diagrams of bath liquid and water washing flow in the implementation of the spinning process, and the condition control capability in the spinning process is represented by CV values. The bath solution concentration CV value is within 1 percent, and the washing flow CV value is controlled within 5 percent.
The embodiments described above are merely preferred embodiments of the present invention, and should not be considered as limitations of the present invention, and features in the embodiments and examples in the present application may be arbitrarily combined with each other without conflict. The protection scope of the present invention is defined by the claims, and includes equivalents of technical features of the claims. I.e., equivalent alterations and modifications within the scope hereof, are also intended to be within the scope of the invention.
Claims (10)
1. The preparation method of the intelligent temperature control type meta-aramid is characterized in that phase change microcapsules are added into a meta-aramid spinning stock solution, and spinning is completed through wet spinning, so that the intelligent temperature control type meta-aramid is obtained, wherein the phase change microcapsules comprise a wall material and a core material wrapped in the wall material, the wall material is poly-p-phenylene terephthalamide, polyurea or polyurethane, the core material is a paraffin/graphene composite material, the paraffin/graphene composite material accounts for 20-75% of the mass of the phase change microcapsules, and the phase change microcapsules account for 3-20% of the mass of the intelligent temperature control type meta-aramid.
2. The method for preparing the intelligent temperature-control meta-aramid fiber as claimed in claim 1, wherein the paraffin in the paraffin/graphene composite material is linear paraffin with a molecular formula CxH2x+2X is more than or equal to 16 and less than or equal to 27; when the wall material adopts poly-p-phenylene terephthamide, the molecular structure is
40≤n≤200。
3. The preparation method of the intelligent temperature-control meta-aramid fiber according to claim 1, wherein the phase-change microcapsule is prepared by an interfacial polymerization method, and the method comprises the following specific steps:
(1) adding an emulsifier into deionized water, stirring and mixing uniformly to form an emulsified solution, and then adding an acid-binding agent to obtain a water phase;
(2) adding a paraffin/graphene composite material and terephthaloyl chloride into an organic solvent, and uniformly stirring and mixing to obtain an organic phase;
(3) and dispersing the uniformly mixed organic phase in a water phase under high-speed stirring, emulsifying, adjusting the stirring speed after the emulsification is finished, adding the prepared p-phenylenediamine solution into the emulsion, finishing the reaction when the pH value of the system is not changed, filtering, washing and drying to obtain the phase-change microcapsule.
4. The preparation method of the intelligent temperature control type meta-aramid fiber as claimed in claim 3, wherein the preparation process of the paraffin/graphene composite material is as follows: heating paraffin at 75 ℃ until the paraffin is completely in a uniform liquid state, adding graphene into the paraffin, stirring for 30-100 min, and then performing ultrasonic oscillation dispersion to obtain a paraffin/graphene composite material; wherein the mass fraction of graphene in the paraffin/graphene composite material is 1-10%.
5. The preparation method of the intelligent temperature-control meta-aramid fiber as claimed in claim 3, wherein the emulsifier in the step (1) is one or two of polyoxyethylene octylphenol ether-10, fatty alcohol polyoxyethylene alkyl ether C12 and polyoxyethylene sorbitan fatty acid ester, and the emulsifying solution contains 5-25 mL of emulsifier per 100mL of emulsifying solution.
6. The preparation method of the intelligent temperature-control meta-aramid fiber according to claim 3, wherein in the step (1), the acid-binding agent is one of sodium hydroxide, calcium hydroxide and sodium bicarbonate; the organic solvent in the step (2) is one of chloroform, diethyl ether, benzene and toluene.
7. The preparation method of the intelligent temperature-control meta-aramid fiber according to claim 3, characterized in that the stirring and mixing time in the step (1) is 15-60 min, and the stirring and mixing time in the step (2) is 30-80 min; and (4) in the step (3), the high-speed stirring speed is 3000-8000 rpm, and the stirring speed is adjusted to be 400-800 rpm after emulsification is finished.
8. The preparation method of the intelligent temperature-control meta-aramid fiber as claimed in claim 3, wherein the mass ratio of the organic phase to the aqueous phase is (85-98): 2-15).
9. The preparation method of the intelligent temperature-control meta-aramid fiber according to claim 3, wherein the molar ratio of the terephthaloyl chloride to the p-phenylenediamine is 1 (1.1-2.2), and the mass concentration of the p-phenylenediamine solution in the step (3) is 5-20%.
10. An intelligent temperature-control meta-aramid fiber, characterized by being prepared by the method for preparing the intelligent temperature-control meta-aramid fiber according to any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110732870.8A CN113584626A (en) | 2021-06-29 | 2021-06-29 | Intelligent temperature control type meta-aramid fiber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110732870.8A CN113584626A (en) | 2021-06-29 | 2021-06-29 | Intelligent temperature control type meta-aramid fiber and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113584626A true CN113584626A (en) | 2021-11-02 |
Family
ID=78245087
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110732870.8A Pending CN113584626A (en) | 2021-06-29 | 2021-06-29 | Intelligent temperature control type meta-aramid fiber and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113584626A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101982231A (en) * | 2010-09-13 | 2011-03-02 | 大连工业大学 | Preparation method of aromatic polyamide core-shell paraffin phase change microcapsule |
| CN102002771A (en) * | 2010-10-21 | 2011-04-06 | 大连工业大学 | Phase-change microcapsule heat storage and temperature adjustment polyacrylonitrile fiber and wet spinning preparation method thereof |
| CN104357021A (en) * | 2014-10-22 | 2015-02-18 | 王子韩 | Graphene/paraffin composite phase change energy storage material and preparation method thereof |
| CN109183179A (en) * | 2018-09-19 | 2019-01-11 | 超美斯新材料（淮安）有限公司 | A kind of preparation method of meta-aramid colored fibre |
-
2021
- 2021-06-29 CN CN202110732870.8A patent/CN113584626A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101982231A (en) * | 2010-09-13 | 2011-03-02 | 大连工业大学 | Preparation method of aromatic polyamide core-shell paraffin phase change microcapsule |
| CN102002771A (en) * | 2010-10-21 | 2011-04-06 | 大连工业大学 | Phase-change microcapsule heat storage and temperature adjustment polyacrylonitrile fiber and wet spinning preparation method thereof |
| CN104357021A (en) * | 2014-10-22 | 2015-02-18 | 王子韩 | Graphene/paraffin composite phase change energy storage material and preparation method thereof |
| CN109183179A (en) * | 2018-09-19 | 2019-01-11 | 超美斯新材料（淮安）有限公司 | A kind of preparation method of meta-aramid colored fibre |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP2046572B1 (en) | Temperature regulating cellulosic fibers and applications thereof | |
| EP1651806B1 (en) | Cellulosic fibers having enhanced reversible thermal properties and methods of forming thereof | |
| US9434869B2 (en) | Cellulosic fibers having enhanced reversible thermal properties and methods of forming thereof | |
| CN108865078A (en) | Phase-change material, yarn, fabric and wearing product for fabric based on microporous barrier | |
| CN108499497A (en) | A kind of graphene microcapsules, intelligent temperature adjusting fiber and preparation method thereof | |
| US11639562B2 (en) | Method for preparing thermal-moisture comfortable polyester FDY | |
| KR102087322B1 (en) | Manufacturing method of core-shell PCM microcapsules with thermostatic function | |
| Karthikeyan et al. | Synthesis, characterization, and development of thermally enhanced cotton fabric using nanoencapsulated phase change materials containing paraffin wax | |
| CN111663214A (en) | Phase-change temperature-regulating fiber blended yarn | |
| CN114481358A (en) | Temperature-adjusting fiber and preparation method thereof | |
| CN114737270A (en) | Phase-change temperature-regulating fiber and preparation method thereof | |
| CN107675278A (en) | A kind of preparation method for the functional fiber element for improving functional materials effective content | |
| CN113584626A (en) | Intelligent temperature control type meta-aramid fiber and preparation method thereof | |
| CN114540972A (en) | Thermochromic fiber and method for preparing thermochromic fabric by using thermochromic fiber | |
| Kamali Moghaddam et al. | Preparation, characterisation and thermal properties of calcium alginate/n-nonadecane microcapsules fabricated by electro-coextrusion for thermo-regulating textiles | |
| CN105908279B (en) | A kind of gloss converts reversible fiber and preparation method thereof | |
| CN117418323B (en) | Multifunctional regenerated cellulose fiber and preparation method and application thereof | |
| Cao et al. | Highly stretchable phase change fibers from coaxial wet spinning of nonaqueous emulsions for temperature regulation | |
| CN102471991B (en) | Production method for modified animal hair fibers | |
| CN106120010A (en) | A kind of clothes of temp. controllable insulation | |
| CN105648578B (en) | Solid-solid phase change composite fibre being crosslinked online with skin-core structure and sandwich layer and preparation method thereof | |
| CN110615898A (en) | Preparation method of high-temperature-resistant alkali-type amino silicone oil emulsion | |
| CN107988648B (en) | Hot and wet comfortable polyester fiber DTY (draw textured yarn) for winter and preparation method thereof | |
| CN114559713A (en) | Unidirectional moisture-conducting and heat-insulating intelligent fabric and preparation method thereof | |
| Wang et al. | Fabrication of air‐conditioning tussah silk with capric–stearic eutectic mixture for effective energy storage and thermal‐regulatory applications |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20211102 |
|
| RJ01 | Rejection of invention patent application after publication |