CN109505027A - Highly sensitive thermally conductive air-conditioning fiber of one kind and preparation method thereof - Google Patents
Highly sensitive thermally conductive air-conditioning fiber of one kind and preparation method thereof Download PDFInfo
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- CN109505027A CN109505027A CN201811446579.9A CN201811446579A CN109505027A CN 109505027 A CN109505027 A CN 109505027A CN 201811446579 A CN201811446579 A CN 201811446579A CN 109505027 A CN109505027 A CN 109505027A
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- 239000000835 fiber Substances 0.000 title claims abstract description 85
- 238000004378 air conditioning Methods 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000012782 phase change material Substances 0.000 claims abstract description 51
- 239000003094 microcapsule Substances 0.000 claims abstract description 31
- 238000002844 melting Methods 0.000 claims abstract description 10
- 230000008018 melting Effects 0.000 claims abstract description 10
- 238000002425 crystallisation Methods 0.000 claims abstract description 8
- 230000008025 crystallization Effects 0.000 claims abstract description 8
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 39
- 238000009987 spinning Methods 0.000 claims description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 30
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 30
- 229910021389 graphene Inorganic materials 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 15
- 206010011732 Cyst Diseases 0.000 claims description 13
- 208000031513 cyst Diseases 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 13
- 229920001807 Urea-formaldehyde Polymers 0.000 claims description 12
- HANVTCGOAROXMV-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine;urea Chemical compound O=C.NC(N)=O.NC1=NC(N)=NC(N)=N1 HANVTCGOAROXMV-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 239000004202 carbamide Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- -1 tertiary amino alkyl ether Chemical class 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 229920000877 Melamine resin Polymers 0.000 claims description 6
- 229920002472 Starch Polymers 0.000 claims description 6
- HOWGUJZVBDQJKV-UHFFFAOYSA-N docosane Chemical compound CCCCCCCCCCCCCCCCCCCCCC HOWGUJZVBDQJKV-UHFFFAOYSA-N 0.000 claims description 6
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 6
- RZJRJXONCZWCBN-UHFFFAOYSA-N octadecane Chemical compound CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 claims description 6
- 239000008107 starch Substances 0.000 claims description 6
- 235000019698 starch Nutrition 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 230000001112 coagulating effect Effects 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 4
- 230000015271 coagulation Effects 0.000 claims description 3
- 238000005345 coagulation Methods 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- 238000002386 leaching Methods 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical group N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims 1
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- 150000005215 alkyl ethers Chemical class 0.000 claims 1
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 229910002804 graphite Inorganic materials 0.000 claims 1
- 239000010439 graphite Substances 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 238000005829 trimerization reaction Methods 0.000 claims 1
- 210000002700 urine Anatomy 0.000 claims 1
- 238000005406 washing Methods 0.000 abstract description 9
- 238000004043 dyeing Methods 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- 239000004744 fabric Substances 0.000 abstract description 4
- 238000007730 finishing process Methods 0.000 abstract description 4
- 230000001788 irregular Effects 0.000 abstract description 4
- 230000004044 response Effects 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 12
- 229920000742 Cotton Polymers 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 239000003995 emulsifying agent Substances 0.000 description 6
- 239000000839 emulsion Substances 0.000 description 6
- 229930040373 Paraformaldehyde Natural products 0.000 description 4
- 239000002202 Polyethylene glycol Substances 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 235000014113 dietary fatty acids Nutrition 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- 229930195729 fatty acid Natural products 0.000 description 4
- 239000000194 fatty acid Substances 0.000 description 4
- 150000004665 fatty acids Chemical class 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229920002866 paraformaldehyde Polymers 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 4
- 229920000053 polysorbate 80 Polymers 0.000 description 4
- 229920000297 Rayon Polymers 0.000 description 3
- 230000006870 function Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003658 microfiber Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000008447 perception Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002964 rayon Substances 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
- 230000028016 temperature homeostasis Effects 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/06—Feeding liquid to the spinning head
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
- D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention provides a kind of highly sensitive thermally conductive air-conditioning fiber, the fiber, and the content of phase-change material micro-capsule is 15.1-17.3%, and melting enthalpy is 35-40J/g, melting temperature is 29-33 DEG C, and crystallization enthalpy is 32-33J/g, and 18-21 DEG C of crystallization range；The present invention also provides the preparation method of above-mentioned fiber, fiber prepared by the present invention, phase-change material micro-capsule is uniformly distributed in the fibre, and is firmly combined with fiber, can be lost to avoid the active principle in fiber with washing or friction；It is found through overtesting, after washing 50 times, the loss late of phase-change material micro-capsule is only 0.1-0.3%；The fabric made of fiber is in finishing process without dyeing defect and irregular phenomenon.Fiber prepared by the present invention, thermal conductivity is in 0.48-0.52W/mK, to being swift in response of ambient temperature, sensitive.
Description
Technical field
The present invention relates to a kind of highly sensitive thermally conductive air-conditioning fibers and preparation method thereof, belong to fibre technology field.
Background technique
The earliest purposes of air-conditioning fiber is developed for making suit, its maximum characteristic is being capable of basis
Extraneous temperature, automatically adjusts the temperature of clothes, and secret is there is the phase transformation with energy conversion function in this fiber
Material can absorb and release incessantly energy to adjust temperature, so that clothes is able to maintain at one comfortably
It just look like that a small air-conditioning is the same, so gaining the name " air-conditioning fiber " in temperature range.
Phase-change material is generally prepared into microcapsules in the prior art, then prepares and adjusts with rayon spinning dope blending spinning
Warm air-conditioning fiber, but have the disadvantage that
(1) existing viscose glue wet spinning, using highly basic strong acid, phase-change material micro-capsule is easy to be destroyed by soda acid, causes damages
Or be lost, it has ruptured and has not been lost the dyeing and finishing process that thoroughly residual phase-change material influences whether fabric, caused dyeing defect and function whole
It manages irregular；
(2) binding force of phase-change material micro-capsule and fiber is not strong, in washing and friction, is easy to be lost, makes the function of fiber
Property be not able to maintain persistently；
(3) temperature-regulating fiber prepared in the prior art, poor to the regulation performance of temperature, there are supercooling, overheat or temperature changes
The small deficiency of amplitude, manufactured finished product snugness of fit are bad.
Summary of the invention
The present invention in order to solve the above technical problems, provides a kind of air-conditioning viscose rayon and preparation method thereof, following to realize
Goal of the invention:
(1) preparation method of fiber of the present invention, phase-change material micro-capsule is lost or loss is few, and the fabric made of fiber exists
Without dyeing defect and irregular phenomenon in finishing process；
(2) air-conditioning fiber prepared by the present invention, water-fastness, abrasion-resistant；
(3) air-conditioning fiber prepared by the present invention, good for the regulation performance of temperature, the perception of ambient temperature is more sensitive, fast
Speed.
In order to solve the above technical problems, The technical solution adopted by the invention is as follows:
A kind of preparation method of air-conditioning fiber, comprising the following steps:
(1) the modified phase-change material micro-capsule of graphene is prepared
A, phase-change material emulsion is prepared
Phase-change material heating is made into its melting, controlled at 85 DEG C, is stirred with the speed of 1200r/min, is then added
It is accounted in the emulsified water of total amount 70% to filling, shears at homogenizer 5000rpm 2 minutes, then dripped with the speed of 4.5ml/min
Add remaining emulsified water, high speed shear 3 minutes at homogenizer 10000rpm prepare phase-change material emulsion.
The mass ratio of phase-change material and emulsified water is 10:26；
The emulsified water has water and emulsifier to be mixed, wherein emulsifier, water mass ratio be 1:24；
The emulsifier is Tween-80；
The phase-change material is made of n-octadecane, polytetramethylene glycol, n-docosane, mass ratio 5:3:1.
, prepare melamine urea-formaldehyde resin cyst material
37% formalin is put into reaction kettle, is stirred, the urea for accounting for total amount 75% is added, adjusting pH value of reaction system is
4,78 DEG C, which are to slowly warm up to, with the speed of 2 DEG C/min reacts 2 hours；Melamine is added, reacts 45 minutes, when performed polymer viscosity
Reach 20s, adjusts pH to 8.5, then addition urea, heat preservation are cooled to 50 DEG C after twenty minutes, starch tertiary amino alkyl ether is added,
It stirs evenly, when being reduced to 35 DEG C, adjusts pH to 7.5, obtain melamine urea-formaldehyde resin cyst material.
The mass ratio of melamine and formaldehyde is 1:32；
The mass ratio of urea and formaldehyde is 1:2.2；
The mass ratio of starch tertiary amino alkyl ether and formaldehyde is 1:10.
, graphene aqueous liquid dispersion preparation
Uniform graphene dispersion solution is obtained by graphene ultrasonic disperse in aqueous solution, after standing；It is added and divides thereto again
Powder-Tween 80 (quality is the 0.3% of graphene A), obtains stable graphene dispersing solution, wherein the concentration of graphene is
0.4wt%.
, polymerization reaction
By phase-change material emulsion in 70 DEG C of water-baths, stirs 15 minutes, melamine urea-formaldehyde resin cyst material is then added dropwise,
It is dripped off within half an hour, citric acid is added dropwise, rate of addition 50ul/s makes system pH be reduced to 4.0, is kept for 20 minutes, is added
Graphene aqueous liquid dispersion；It then proceedes to that citric acid is added dropwise, 25 ul/s of rate of addition reduces pH to 2-3 and stops being added dropwise, is added dropwise
It is 500r/min that process, which is kept stirring revolving speed, is then warming up to 80 DEG C, is solidified 2 hours, stands, supernatant liquor is poured out, water is added
Washing is filtered, is repeated 2 times, and vacuum drying obtains the modified phase-change material micro-capsule of graphene.
The quality of the graphene is the 0.9% of phase-change material quality；
The partial size D97 of the phase-change material micro-capsule is 1-2 μm.
The mass ratio of the melamine urea-formaldehyde resin cyst material and phase-change material is 1:4.
(2) spinning solution is prepared
Cotton Pulp and paraformaldehyde, DMSO are added in reaction kettle, are heated to 125 DEG C, speed of agitator 2000r/min, dissolution 1
Hour, 105 DEG C, speed of agitator 600r/min are then cooled to, is dissolved 1 hour, is then stood vacuum through filtering, room temperature and take off
Spinning solution is made in bubble；
The Cotton Pulp, pH 6.8-7, DP 550.
The mass ratio of the Cotton Pulp and paraformaldehyde, DMSO is 1:0.7:20；
The spinning solution, viscosity 180s, the content of alpha cellulose are 4.6%；
Course of dissolution needs continuous air extraction, recycles formaldehyde extra in kettle；
The standing vacuum defoamation, time are 13 hours.
(3) co-blended spinning liquid is prepared
The modified phase-change material micro-capsule of graphene is added in spinning solution, fatty acid polyethylene glycol ester is added, is stirred
Uniformly, co-blended spinning liquid is prepared；
The mass ratio of fatty acid polyethylene glycol ester and spinning solution is 1:25；
The mass ratio of alpha cellulose is 0.175:1 in the phase-change material micro-capsule and spinning solution.
(4) spinning moulding
Co-blended spinning liquid is added to the coagulating bath adjusted and carries out spinning, is stirred evenly, the coagulating bath is the aqueous solution of DMSO,
Wherein the concentration of DMSO is 28%；Coagulation bath temperature is 35 DEG C；Leaching length: 700 millimeters, spray head drawing-off: -3.5%；Drawing-off 18% between disk,
Two bath drawing-offs 33%, three bath drawing-offs 27%, spin speed 32m/min；Two baths, coolant-temperature gage are 55 DEG C, and three baths, coolant-temperature gage is 70 DEG C.
Melamine urea-formaldehyde resin cyst material prepared by the present invention prepares micro- glue in addition to can be used for coating phase-change material
Capsule, while preferably can also firmly be combined with fiber, prevent the loss or loss of microcapsules.
Graphene can assign fiber good thermal conductivity, and the present invention uses the ratio of specific graphene and phase-change material
Example, in conjunction with the type and proportion and phase-change material micro-capsule of phase-change material and the ratio of cellulose, so that the air-conditioning of preparation is fine
The thermoregulation effect of dimension is more preferable.
Above technical scheme is used, the invention has the benefit that
(1) fiber prepared by the present invention, the content of phase-change material micro-capsule is 15.1-17.3% in fiber, and melting enthalpy is 35-
40J/g, melting temperature be 29-33 DEG C, crystallization enthalpy be 32-33J/g, 18-21 DEG C of crystallization range.
(2) fiber prepared by the present invention, phase-change material micro-capsule are uniformly distributed in the fibre, and firm with the combination of fiber
Gu and can to avoid fiber active principle with washing or friction be lost；It is found through overtesting, after washing 50 times, phase transformation material
The loss late for expecting microcapsules is only 0.1-0.3%；The fabric made of fiber is in finishing process without dyeing defect and irregular phenomenon.
(3) fiber prepared by the present invention, thermal conductivity is in 0.48-0.52W/mK, to being swift in response of ambient temperature, sensitive.
The temperature rise period for being 20 ~ 40 DEG C in environment temperature, air-conditioning fiber start to absorb heat, itself heating rate at 29 DEG C
It slows down gradually.When environment temperature is 31 DEG C, the general fibre temperature difference under air-conditioning fiber prepared by the present invention and similarity condition is maximum,
6.5-7 DEG C lower than the temperature of general fibre；In the temperature-rise period that environment temperature is 29-33 DEG C, air-conditioning fiber prepared by the present invention
It is low 5 DEG C average than general fibre；In the temperature-rise period that environment temperature is 34-40 DEG C, air-conditioning fiber prepared by the present invention is than common
Fiber is low 2.5 DEG C average；Under 40 degrees Celsius of environment temperatures, after 1 hour, temperature progressivelyes reach environment temperature.
The temperature-fall period for being 40 ~ 10 DEG C in environment temperature, air-conditioning fiber prepared by the present invention start to discharge heat at 21 DEG C,
Itself rate of temperature fall slows down gradually.When environment temperature is 20 DEG C, air-conditioning fiber prepared by the present invention is compared with general fibre, the temperature difference
Maximum is 5.5-6 DEG C higher than the temperature of general fibre；During the decline that environment temperature is 21-18 DEG C, air-conditioning prepared by the present invention
Fiber is than 4 DEG C of general fibre mean height, during the decline that environment temperature is 17-10 DEG C, air-conditioning fiber ratio prepared by the present invention
2 DEG C of general fibre mean height.Under 10 degrees Celsius of environment temperatures, after 1 hour, temperature progressivelyes reach environment temperature.
(4) phase-changing and temperature-regulating fiber prepared by the present invention, fiber number 1.9dtex, doing breaking strength is 2.82-2.84cN/
Dtex, dry elongation at break are 17.8-18.1%, and hook is 0.74-0.77 cN/dtex by force.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described, it should be understood that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
A kind of preparation method of the air-conditioning fiber of embodiment 1, comprising the following steps:
(1) the modified phase-change material micro-capsule of graphene is prepared
A, phase-change material emulsion is prepared
Phase-change material heating is made into its melting, controlled at 85 DEG C, is stirred with the speed of 1200r/min, is then added
It is accounted in the emulsified water of total amount 70% to filling, shears at homogenizer 5000rpm 2 minutes, then dripped with the speed of 4.5ml/min
Add remaining emulsified water, high speed shear 3 minutes at homogenizer 10000rpm prepare phase-change material emulsion.
The mass ratio of phase-change material and emulsified water is 10:26；
The emulsified water has water and emulsifier to be mixed, wherein emulsifier, water mass ratio be 1:24；
The emulsifier is Tween-80；
The phase-change material is made of n-octadecane, polytetramethylene glycol, n-docosane, mass ratio 5:3:1.
, prepare melamine urea-formaldehyde resin cyst material
37% formalin is put into reaction kettle, is stirred, the urea for accounting for total amount 75% is added, adjusting pH value of reaction system is
4,78 DEG C, which are to slowly warm up to, with the speed of 2 DEG C/min reacts 2 hours；Melamine is added, reacts 45 minutes, when performed polymer viscosity
Reach 20s, adjusts pH to 8.5, then addition urea, heat preservation are cooled to 50 DEG C after twenty minutes, starch tertiary amino alkyl ether is added,
It stirs evenly, when being reduced to 35 DEG C, adjusts pH to 7.5, obtain melamine urea-formaldehyde resin cyst material.
The mass ratio of melamine and formaldehyde is 1:32；
The mass ratio of urea and formaldehyde is 1:2.2；
The mass ratio of starch tertiary amino alkyl ether and formaldehyde is 1:10.
, graphene aqueous liquid dispersion preparation
Uniform graphene dispersion solution is obtained by graphene ultrasonic disperse in aqueous solution, after standing；It is added and divides thereto again
Powder-Tween 80 (quality is the 0.3% of graphene A), obtains stable graphene dispersing solution, wherein the concentration of graphene is
0.4wt%.
, polymerization reaction
By phase-change material emulsion in 70 DEG C of water-baths, stirs 15 minutes, melamine urea-formaldehyde resin cyst material is then added dropwise,
It is dripped off within half an hour, citric acid is added dropwise, rate of addition 50ul/s makes system pH be reduced to 4.0, is kept for 20 minutes, is added
Graphene aqueous liquid dispersion；It then proceedes to that citric acid is added dropwise, 25 ul/s of rate of addition reduces pH to 2-3 and stops being added dropwise, is added dropwise
It is 500r/min that process, which is kept stirring revolving speed, is then warming up to 80 DEG C, is solidified 2 hours, stands, supernatant liquor is poured out, water is added
Washing is filtered, is repeated 2 times, and vacuum drying obtains the modified phase-change material micro-capsule of graphene.
The quality of the graphene is the 0.9% of phase-change material quality；
The partial size D97 of the phase-change material micro-capsule is 1-2 μm.
The mass ratio of the melamine urea-formaldehyde resin cyst material and phase-change material is 1:4.
(2) spinning solution is prepared
Cotton Pulp and paraformaldehyde, DMSO are added in reaction kettle, are heated to 125 DEG C, speed of agitator 2000r/min, dissolution 1
Hour, 105 DEG C, speed of agitator 600r/min are then cooled to, is dissolved 1 hour, is then stood vacuum through filtering, room temperature and take off
Spinning solution is made in bubble；
The Cotton Pulp, pH 6.8-7, DP 550.
The mass ratio of the Cotton Pulp and paraformaldehyde, DMSO is 1:0.7:20；
The spinning solution, viscosity 180s, the content of alpha cellulose are 4.6%；
Course of dissolution needs continuous air extraction, recycles formaldehyde extra in kettle；
The standing vacuum defoamation, time are 13 hours.
(3) co-blended spinning liquid is prepared
The modified phase-change material micro-capsule of graphene is added in spinning solution, fatty acid polyethylene glycol ester is added, is stirred
Uniformly, co-blended spinning liquid is prepared；
The mass ratio of fatty acid polyethylene glycol ester and spinning solution is 1:25；
The mass ratio of alpha cellulose is 0.175:1 in the phase-change material micro-capsule and spinning solution.
(4) spinning moulding
Co-blended spinning liquid is added to the coagulating bath adjusted and carries out spinning, the coagulating bath is the aqueous solution of DMSO, wherein DMSO
Concentration be 28%；Coagulation bath temperature is 35 DEG C；Leaching length: 700 millimeters, spray head drawing-off: -3.5%；Drawing-off 18% between disk, two bath drawing-offs
33%, speed 32m/min is spun in three bath drawing-offs 27%；Two baths, coolant-temperature gage are 55 DEG C, and three baths, coolant-temperature gage is 70 DEG C.
(1) fiber prepared by the present invention, the content of phase-change material micro-capsule is 15.1-17.3% in fiber, and melting enthalpy is
35-40J/g, melting temperature be 29-33 DEG C, crystallization enthalpy be 32-33J/g, 18-21 DEG C of crystallization range.
(2) fiber prepared by the present invention, phase-change material micro-capsule are uniformly distributed in the fibre, and firm with the combination of fiber
Gu and can be lost to avoid the active principle in fiber with washing or friction；It is found through overtesting, after washing 50 times, phase transformation
The loss late of material microcapsule is only 0.1-0.3%.
The temperature rise period for being 20 ~ 40 DEG C in environment temperature, air-conditioning fiber start to absorb heat, itself heating rate at 29 DEG C
It slows down gradually.When environment temperature is 31 DEG C, the general fibre temperature difference under air-conditioning fiber prepared by the present invention and similarity condition is maximum,
6.5-7 DEG C lower than the temperature of general fibre；In the temperature-rise period that environment temperature is 29-33 DEG C, air-conditioning fiber prepared by the present invention
It is low 5 DEG C average than general fibre；In the temperature-rise period that environment temperature is 34-40 DEG C, air-conditioning fiber prepared by the present invention is than common
Fiber is low 2.5 DEG C average；
The temperature-fall period for being 40 ~ 10 DEG C in environment temperature, air-conditioning fiber prepared by the present invention start to discharge heat at 21 DEG C, itself
Rate of temperature fall slows down gradually.When environment temperature is 20 DEG C, air-conditioning fiber prepared by the present invention is compared with general fibre, and the temperature difference is most
Greatly, 5.5-6 DEG C higher than the temperature of general fibre；During the decline that environment temperature is 21-18 DEG C, air-conditioning prepared by the present invention is fine
Dimension is than 4 DEG C of general fibre mean height, and during the decline that environment temperature is 17-10 DEG C, air-conditioning fiber prepared by the present invention is than general
2 DEG C of perforating fiber mean height.
(3) phase-changing and temperature-regulating fiber prepared by the present invention, fiber number 1.9dtex, doing breaking strength is 2.82-2.84cN/
Dtex, dry elongation at break are 17.8-18.1%, and hook is 0.74-0.77 cN/dtex by force.
Unless otherwise indicated, percentage employed in the present invention is mass percent.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (8)
1. a kind of highly sensitive thermally conductive air-conditioning fiber, it is characterised in that: the fiber, the content of phase-change material micro-capsule are 15.1-
17.3%, melting enthalpy is 35-40J/g, melting temperature is 29-33 DEG C, and crystallization enthalpy is 32-33J/g, crystallization range 18-
21℃。
2. the highly sensitive thermally conductive air-conditioning fiber of one kind according to claim 1, it is characterised in that: the fiber, thermal conductivity exist
0.48-0.52W/mK。
3. a kind of preparation method of highly sensitive thermally conductive air-conditioning fiber, it is characterised in that: the preparation method, including prepare graphene
Modified phase-change material micro-capsule prepares co-blended spinning liquid, spinning moulding；
It is described to prepare the modified phase-change material micro-capsule of graphene, including prepare melamine urea-formaldehyde resin cyst material.
4. the preparation method of the highly sensitive thermally conductive air-conditioning fiber of one kind according to claim 3, it is characterised in that: the preparation
Melamine urea-formaldehyde resin cyst material puts into 37% formalin in reaction kettle, and the urine for accounting for total amount 75% is added in stirring
Element, adjusting pH value of reaction system is 4, is warming up to 78 DEG C and reacts 2 hours；Melamine is added, reacts 45 minutes, when performed polymer is viscous
Degree reaches 20s, adjusts pH to 8.5, remaining urea is then added, heat preservation is cooled to 50 DEG C after twenty minutes, addition starch tertiary ammonia
Base alkyl ether, stirs evenly, and when being reduced to 35 DEG C, adjusts pH to 7.5, obtains melamine urea-formaldehyde resin cyst material.
5. the preparation method of the highly sensitive thermally conductive air-conditioning fiber of one kind according to claim 4, it is characterised in that: the trimerization
The mass ratio of cyanamide and formaldehyde is 1:32；The mass ratio of urea and formaldehyde is 1:2.2；Starch tertiary amino alkyl ether and formaldehyde
Mass ratio is 1:10.
6. the preparation method of the highly sensitive thermally conductive air-conditioning fiber of one kind according to claim 3, it is characterised in that: the preparation
The modified phase-change material micro-capsule of graphene is added in spinning solution, prepares co-blended spinning liquid by co-blended spinning liquid；The graphite
The mass ratio of alpha cellulose is 0.175:1 in alkene modified phase-change material micro-capsule and spinning solution.
7. the preparation method of the highly sensitive thermally conductive air-conditioning fiber of one kind according to claim 6, it is characterised in that: the spinning
Stoste, viscosity 180s, the content of alpha cellulose are 4.6%；
The modified phase-change material micro-capsule of the graphene, the quality of graphene are the 0.9% of phase-change material quality；Melamine
The mass ratio of Lauxite cyst material and phase-change material is 1:4；
The phase-change material is made of n-octadecane, polytetramethylene glycol, n-docosane, mass ratio 5:3:1.
8. the preparation method of the highly sensitive thermally conductive air-conditioning fiber of one kind according to claim 3, it is characterised in that: the spinning
Molding, the coagulating bath are the aqueous solution of DMSO, and wherein the concentration of DMSO is 28%；Coagulation bath temperature is 35 DEG C；Leaching length: 700 millis
Rice, spray head drawing-off: -3.5%；Speed 32m/min is spun in drawing-off 18% between disk, two bath drawing-offs 33%, three bath drawing-offs 27%；Two baths, coolant-temperature gage
It is 55 DEG C, three baths, coolant-temperature gage is 70 DEG C.
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