CN104928781B - A kind of preparation method of the energy-saving and temperature-regulating fiber with far-infrared functional - Google Patents
A kind of preparation method of the energy-saving and temperature-regulating fiber with far-infrared functional Download PDFInfo
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Abstract
The invention provides a kind of preparation method of the energy-saving and temperature-regulating fiber with far-infrared functional, it is characterised in that including：Step 1：Porous nano powder, Triallyl isocyanurate, polyethyleneglycol diacrylate, polyethylene glycol, nano aluminum Magnesium coumpoud oxide and initiator are placed in aqueous solvent, using the scattered method of depressurizing ultrasonic, reacted at 65 75 DEG C 2~5 hours, most obtain far infrared energy storage phase change material after centrifugal dehydration afterwards；Step 2：By above-mentioned far infrared energy storage phase change material through dried process after, be blended through twin-screw with polymer chips and granulated, then the energy-saving and temperature-regulating fiber with far-infrared functional is obtained through melt spinning, wherein 260 DEG C~315 DEG C of spinning temperature spins 800~3500m/min of speed.Far infrared phase-changing energy storage material prepared by the present invention has the advantages that energy storage temperature control ability is strong, preparation cost is low, heat-resistant stability good, simple to operate.
Description
Technical field
The invention belongs to the preparation field of far infrared intelligent temperature-regulating fiber, more particularly to a kind of storage with far-infrared functional
The preparation method of energy temperature-regulating fiber.
Background technology
Phase-change energy-storage temperature adjustment fiber is to develop a kind of high technical fibre faster in recent years, can be by the external micro- sky of regulation
Between environment temperature reach the purpose of energy storage temperature control.Because microencapsulated phase change material heat resistance is poor, blending phase-change material is easy
The problem of leakage, current polyester fiber, the exploitation of the energy storage temperature controlling function of Fypro are very restricted.Far infrared is fine
Dimension is a kind of functional fibre containing far infrared powder.By absorbing far infrared, body surface's skin can occur special life
Reason change, produces warming, health care the function that heats up.It is low, compatible by far infrared addition diameter of particle size heterogeneity, transmission power
The reasons such as property difference, far-infrared polyester, the exploitation of Fypro also receive certain limitation.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the energy-saving and temperature-regulating fiber with far-infrared functional, the method is
Phase change medium and far-infrared functional powder are loaded using the pore space structure of nano-powder, it is sealed using crosslinking agent then
Dress, the characteristics of the far infrared phase-change material of preparation both has similar microcapsule structure, with enthalpy of phase change higher and higher remote red
Emission power, shows the advantage of high thermal stability again；Far infrared phase-changing energy storage material of the invention can preferably be applied to
A series of modified field of the multifunction of the general fiber of high-melting-points such as polyester, polyamide.
In order to achieve the above object, the invention provides a kind of preparation side of the energy-saving and temperature-regulating fiber with far-infrared functional
Method, it is characterised in that including：
Step 1：By porous nano powder, Triallyl isocyanurate, polyethyleneglycol diacrylate, polyethylene glycol,
Nano aluminum Magnesium coumpoud oxide and initiator are placed in aqueous solvent, using the scattered method of depressurizing ultrasonic, are reacted at 65-75 DEG C
2~5 hours, far infrared energy storage phase change material is most obtained after centrifugal dehydration afterwards；
Step 2：By above-mentioned far infrared energy storage phase change material through dried process after, with polymer chips through double screw extruder
Blending granulation, then obtain the energy-saving and temperature-regulating fiber with far-infrared functional, wherein spinning temperature 260 DEG C~315 through melt spinning
DEG C, spin 800~3500m/min of speed.
Preferably, described porous nano powder, Triallyl isocyanurate, polyethyleneglycol diacrylate, nanometer
The w/v of magnalium composite oxides, initiator, polyethylene glycol and aqueous solvent is：30~60g: 5~10g: 5~10g: 10
~20g: 0.1~1g: 19.9~49.9g: 200mL.
Preferably, the number-average molecular weight of described polyethylene glycol is 1000~6000.
Preferably, described nano aluminum Magnesium coumpoud oxide particle diameter is 10~300nm.
Preferably, described step 2 mid and far infrared energy storage phase change material and the mass ratio 5: 95~30 with polymer chips:
70,240 DEG C~305 DEG C of prilling temperature.
Preferably, described porous nano powder be porous silica, aeroge and diatomite in one or two
It is composited, the particle diameter of porous nano powder is 300~600nm.
Preferably, described polymer chips is polyethylene terephthalate, PTT, gathers
In mutual-phenenyl two acid bromide two alcohol ester, PEN, polyamide 6, polyamide 66, polyamide 56 and polyamide 1010
One kind.
It is contemplated that prepare it is a kind of both there is energy-storage thermal-insulating function, while have the multifunctional fibre of far-infrared functional concurrently,
Thinking is provided for the multifunction of polyester, Fypro is modified.It is carrier substrate that the present invention chooses inorganic nanometer powder first,
The inside that energy storage phase change medium polyethylene glycol high, far infrared nano powder are loaded into inorganic particle by the method for ultrasound decompression is empty
In gap, nano-particle is packaged using crosslinking agent Triallyl isocyanurate, polyethyleneglycol diacrylate then, such as
Shown in Fig. 1.In addition, ultrasonication can not only prevent the reunion of nano particle, the carrying out of reaction can be promoted again.By said structure
And the design of technique, the energy storage of the dispersiveness, phase-change material of nano particle can not only be ensured, also make phase-change material that there is height
Heat endurance, far-infrared transmitting function, to realize that dystectic far infrared energy-storage thermal-insulating fibre forming such as polyester, polyamide is provided
A kind of new means.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) far infrared phase-changing energy storage material prepared by the present invention have that energy storage temperature control ability is strong, preparation cost is low, it is heat-resisting steady
Qualitative good, simple to operate advantage.
(2) far infrared energy-saving and temperature-regulating fiber prepared by the present invention, its far-infrared functional can be realized with energy storage temperature controlling function
Have complementary advantages, mutually support.Phase-change material can provide energy for far infrared powder, after being stimulated by far infrared, body surface temperature
The rising of degree, can promote the energy-saving and temperature-regulating ability of phase-change material again.
(3) far infrared phase-changing energy storage material prepared by the present invention can be applied preferably in high-melting-points such as polyester, polyamide
The modified aspect of the multifunction of polymer.
Brief description of the drawings
Fig. 1 is the schematic flow sheet that the inventive method prepares far infrared intelligent temperature adjustment phase-change material.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Nano aluminum Magnesium coumpoud oxide described in various embodiments of the present invention is prepared with reference to patent of invention CN 102776600B,
Particle diameter is 10~300nm.
Polyethyleneglycol diacrylate described in various embodiments of the present invention is purchased from lark prestige Science and Technology Ltd., and its number is divided equally
Son amount is 250~750.
Azo-bis-isobutyrate hydrochloride of the present invention is purchased from Qingdao Runxing Photoelectric Material Co., Ltd., trade mark V50.
Phase transformation enthalpy in various embodiments of the present invention is determined by DSC and obtained.
Embodiment 1
A kind of preparation method of the energy-saving and temperature-regulating fiber with far-infrared functional, concretely comprises the following steps：
First, by the porous silica (length is about 300nm) of 30g, the Triallyl isocyanurate of 10g, 10g
Polyethyleneglycol diacrylate, the nano aluminum Magnesium coumpoud oxide of 10g, the initiator (ammonium persulfate) of 1g, the polyethylene glycol of 39g
(number-average molecular weight is about 1000) is added in 200ml deionized waters, using the scattered method of depressurizing ultrasonic (pressure 200Pa~
500Pa, 20~40KHz of supersonic frequency), it is warming up to 70 DEG C and reacts 5 hours.Far infrared energy-saving and temperature-regulating phase is obtained after centrifugal dehydration
Become material, it is standby through 80 DEG C of dryings 12 hours.
By the poliester chip of the far infrared phase-change material of the 30g of dried process and 70g through double spiral shells
The 260 DEG C of blending granulations of bar extruder, and obtain the energy-saving and temperature-regulating fiber with far-infrared functional, wherein spinning through melt spinning machine
280 DEG C of temperature, spins speed 800m/min.Find after tested, the phase transformation enthalpy for preparing fiber reaches 15~25J/g, far infrared transmission
Rate 75%.
Embodiment 2
A kind of preparation method of the energy-saving and temperature-regulating fiber with far-infrared functional, concretely comprises the following steps：
First, by the diatomite (length is about 600nm) of 40g, the Triallyl isocyanurate of 5g, 5g polyethylene glycol
Diacrylate, the nano aluminum Magnesium coumpoud oxide of 10g, the initiator (azo-bis-isobutyrate hydrochloride) of 0.1g, 39.9g it is poly-
Ethylene glycol (number-average molecular weight is about 6000) is added in 200ml deionized waters, using the scattered method of depressurizing ultrasonic, (pressure
200Pa~500Pa, 20~40KHz of supersonic frequency), it is warming up to 70 DEG C and reacts 2 hours.Far infrared storage is obtained after centrifugal dehydration
Can temperature adjustment phase-change material, it is standby through 80 DEG C of dryings 12 hours.
The PTT of the far infrared phase-change material of the 5g of dried process and 95g is cut into slices through twin-screw
270 DEG C of blending granulations of extruder, and obtain the energy-saving and temperature-regulating fiber with far-infrared functional, wherein spinning temperature through melt spinning machine
290 DEG C of degree, spins speed 3500m/min.Find after tested, the phase transformation enthalpy for preparing fiber reaches 15~25J/g, far infrared transmissivity
70%.
Embodiment 3
A kind of preparation method of the energy-saving and temperature-regulating fiber with far-infrared functional, concretely comprises the following steps：
First, by the porous silica (length is about 600nm) of 20g, the diatomite (length is about 600nm) of 20g, 5g
Triallyl isocyanurate, the polyethyleneglycol diacrylate of 5g, the nano aluminum Magnesium coumpoud oxide of 10g, the initiation of 1g
Agent (azo-bis-isobutyrate hydrochloride), the polyethylene glycol (number-average molecular weight is about 2000) of 39g are added to 200ml deionized waters
In, using the scattered method of depressurizing ultrasonic (pressure 200Pa~500Pa, 20~40KHz of supersonic frequency), it is warming up to 70 DEG C of reactions 4
Hour.Far infrared energy-saving and temperature-regulating phase-change material is obtained after centrifugal dehydration, it is standby through 80 DEG C of dryings 12 hours.
The PEN of the far infrared phase-change material of the 10g of dried process and 90g is cut into slices through twin-screw
305 DEG C of blending granulations of extruder, and obtain the energy-saving and temperature-regulating fiber with far-infrared functional, wherein spinning temperature through melt spinning machine
315 DEG C of degree, spins speed 1000m/min.Find after tested, the phase transformation enthalpy for preparing fiber reaches 15~25J/g, far infrared transmissivity
75%.
Embodiment 4
A kind of preparation method of the energy-saving and temperature-regulating fiber with far-infrared functional, concretely comprises the following steps：
First, by the porous silica (length is about 600nm) of 15g, the diatomite (length is about 600nm) of 15g,
The Triallyl isocyanurate of 10g, the polyethyleneglycol diacrylate of 5g, the nano aluminum Magnesium coumpoud oxide of 20g, 1g draw
Hair agent (ammonium persulfate), the polyethylene glycol (number-average molecular weight is about 2000) of 34g are added in 200ml deionized waters, using subtracting
The method (pressure 200Pa~500Pa, 20~40KHz of supersonic frequency) of ultrasonic disperse is pressed, 70 DEG C is warming up to and is reacted 4 hours.Through from
Far infrared energy-saving and temperature-regulating phase-change material is obtained after heart dehydration, it is standby through 80 DEG C of dryings 12 hours.
The phase-change material of the 20g of dried process is made with the polyamide section of 80g through 240 DEG C of blendings of double screw extruder
Grain, and the energy-saving and temperature-regulating fiber with far-infrared functional, wherein 260 DEG C of spinning temperature are obtained through melt spinning machine, spin speed 800m/
min.Find after tested, the phase transformation enthalpy for preparing fiber reaches 15~25J/g, far infrared transmissivity 75%.
Claims (7)
1. a kind of preparation method of the energy-saving and temperature-regulating fiber with far-infrared functional, it is characterised in that including：
Step 1：By porous nano powder, Triallyl isocyanurate, polyethyleneglycol diacrylate, polyethylene glycol, nanometer
Magnalium composite oxides and initiator are placed in aqueous solvent, using the scattered method of depressurizing ultrasonic, 2 ~ 5 are reacted at 65-75 DEG C
Hour, far infrared energy storage phase change material is most obtained after centrifugal dehydration afterwards；
Step 2：By above-mentioned far infrared energy storage phase change material through dried process after, with polymer chips through double screw extruder be blended
Granulation, then the energy-saving and temperature-regulating fiber with far-infrared functional, wherein 260 DEG C ~ 315 DEG C of spinning temperature are obtained through melt spinning, spin
800 ~ 3500 m/min of speed.
2. there is the preparation method of the energy-saving and temperature-regulating fiber of far-infrared functional as claimed in claim 1, it is characterised in that described
Porous nano powder, Triallyl isocyanurate, polyethyleneglycol diacrylate, nano aluminum Magnesium coumpoud oxide, trigger
The w/v of agent, polyethylene glycol and aqueous solvent is：30~60g：5~10g：5~10 g：10~20 g：0.1~1g：19.9~
49.9 g：200mL.
3. there is the preparation method of the energy-saving and temperature-regulating fiber of far-infrared functional as claimed in claim 1, it is characterised in that described
Polyethylene glycol number-average molecular weight be 1000 ~ 6000.
4. there is the preparation method of the energy-saving and temperature-regulating fiber of far-infrared functional as claimed in claim 1, it is characterised in that described
Nano aluminum Magnesium coumpoud oxide particle diameter be 10 ~ 300 nm.
5. there is the preparation method of the energy-saving and temperature-regulating fiber of far-infrared functional as claimed in claim 1, it is characterised in that described
The step of 2 mid and far infrared energy storage phase change materials and polymer chips mass ratio 5:95~30:70, prilling temperature 240 DEG C ~ 305
℃。
6. there is the preparation method of the energy-saving and temperature-regulating fiber of far-infrared functional as claimed in claim 1, it is characterised in that described
Porous nano powder be composited for one or two in porous silica and diatomite, the particle diameter of porous nano powder
It is 300 ~ 600 nm.
7. there is the preparation method of the energy-saving and temperature-regulating fiber of far-infrared functional as claimed in claim 1, it is characterised in that described
Polymer chips for polyethylene terephthalate, PTT, polybutylene terephthalate (PBT),
One kind in PEN, polyamide 6, polyamide 66, polyamide 56 and polyamide 1010.
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| CN106749971B (en) * | 2016-12-07 | 2018-10-12 | 大连工业大学 | A kind of preparation method for the phase-change accumulation energy solution being used to prepare phase transformation viscose rayon |
| CN107142546B (en) * | 2017-06-07 | 2018-06-01 | 广州市中诚新型材料科技有限公司 | The compound polyester functional fibre of a kind of far infrared, antibacterial mite-removing and its manufacturing method |
| CN108588871B (en) * | 2018-04-26 | 2020-12-18 | 东华大学 | Preparation method for preparing special-shaped high-strength polyamide 6 fiber by near-infrared light induced drafting |
| CN110451860B (en) * | 2019-08-26 | 2021-08-31 | 厦门美益兴业建材有限公司 | Energy-saving high-temperature-resistant concrete and preparation method thereof |
| US11306238B2 (en) | 2019-10-03 | 2022-04-19 | King Fahd University Of Petroleum And Minerals | Shape-stabilized phase change materials for energy storage |
| CN110735198A (en) * | 2019-11-29 | 2020-01-31 | 福建六树网络科技有限公司 | modified PET polyester fiber, preparation method thereof and polyester fabric |
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| CN100381621C (en) * | 2006-08-16 | 2008-04-16 | 四川大学 | Method of in situ encapsulation preparing phase-change energy-storage fibre |
| CN100489187C (en) * | 2007-05-30 | 2009-05-20 | 天津工业大学 | Intelligent temperature-regulation fabric and preparing method |
| CN101451307A (en) * | 2007-12-06 | 2009-06-10 | 华楙生化科技股份有限公司 | Long acting cooling composite powder, cooling fiber and method for producing the same |
| CN101392461B (en) * | 2008-10-15 | 2010-09-01 | 清华大学深圳研究生院 | Phase change energy storage low temperature face mask substrate material and preparation method thereof |
| KR20100070917A (en) * | 2008-12-18 | 2010-06-28 | 제일모직주식회사 | Phase change material- aerogel complex and method for preparing thereof |
| CN102443878B (en) * | 2011-09-23 | 2014-01-15 | 大连工业大学 | Multifunctional comfort fiber with functions of phase transition temperature regulation, moisture absorption and moisture wicking |
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| CN103243406B (en) * | 2013-05-22 | 2015-05-27 | 东华大学 | Method for preparing intelligent temperature regulation fiber by melt spinning process |
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