CN105648578B - Solid-solid phase change composite fibre being crosslinked online with skin-core structure and sandwich layer and preparation method thereof - Google Patents
Solid-solid phase change composite fibre being crosslinked online with skin-core structure and sandwich layer and preparation method thereof Download PDFInfo
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- CN105648578B CN105648578B CN201610012846.6A CN201610012846A CN105648578B CN 105648578 B CN105648578 B CN 105648578B CN 201610012846 A CN201610012846 A CN 201610012846A CN 105648578 B CN105648578 B CN 105648578B
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- 239000000835 fiber Substances 0.000 title claims abstract description 91
- 239000002131 composite material Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 52
- 239000007790 solid phase Substances 0.000 title claims abstract description 7
- 230000008859 change Effects 0.000 title abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 24
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 23
- 239000010695 polyglycol Substances 0.000 claims abstract description 23
- 229920000151 polyglycol Polymers 0.000 claims abstract description 23
- 239000003999 initiator Substances 0.000 claims abstract description 21
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000004132 cross linking Methods 0.000 claims abstract description 18
- 235000010443 alginic acid Nutrition 0.000 claims abstract description 8
- 229920000615 alginic acid Polymers 0.000 claims abstract description 8
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229940072056 alginate Drugs 0.000 claims abstract description 7
- 238000005516 engineering process Methods 0.000 claims abstract description 6
- 238000012805 post-processing Methods 0.000 claims abstract description 3
- 238000002166 wet spinning Methods 0.000 claims abstract description 3
- 239000012782 phase change material Substances 0.000 claims description 47
- 239000011162 core material Substances 0.000 claims description 41
- 238000009987 spinning Methods 0.000 claims description 38
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 37
- 235000010413 sodium alginate Nutrition 0.000 claims description 37
- 239000000661 sodium alginate Substances 0.000 claims description 37
- 229940005550 sodium alginate Drugs 0.000 claims description 37
- 239000007787 solid Substances 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 16
- 230000001112 coagulating effect Effects 0.000 claims description 15
- 238000007493 shaping process Methods 0.000 claims description 15
- 238000002844 melting Methods 0.000 claims description 12
- 230000008018 melting Effects 0.000 claims description 12
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 11
- 239000001110 calcium chloride Substances 0.000 claims description 11
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000013019 agitation Methods 0.000 claims description 10
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 3
- 239000003431 cross linking reagent Substances 0.000 claims description 3
- 230000007704 transition Effects 0.000 claims description 3
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical group C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 abstract description 25
- 230000008025 crystallization Effects 0.000 abstract description 25
- 238000004146 energy storage Methods 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 53
- 239000012071 phase Substances 0.000 description 18
- 239000004743 Polypropylene Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000002135 phase contrast microscopy Methods 0.000 description 4
- -1 polypropylene Polymers 0.000 description 4
- 229920001155 polypropylene Polymers 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- 239000004744 fabric Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 206010054949 Metaplasia Diseases 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 235000010410 calcium alginate Nutrition 0.000 description 1
- 239000000648 calcium alginate Substances 0.000 description 1
- 229960002681 calcium alginate Drugs 0.000 description 1
- OKHHGHGGPDJQHR-YMOPUZKJSA-L calcium;(2s,3s,4s,5s,6r)-6-[(2r,3s,4r,5s,6r)-2-carboxy-6-[(2r,3s,4r,5s,6r)-2-carboxylato-4,5,6-trihydroxyoxan-3-yl]oxy-4,5-dihydroxyoxan-3-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylate Chemical compound [Ca+2].O[C@@H]1[C@H](O)[C@H](O)O[C@@H](C([O-])=O)[C@H]1O[C@H]1[C@@H](O)[C@@H](O)[C@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@H](O2)C([O-])=O)O)[C@H](C(O)=O)O1 OKHHGHGGPDJQHR-YMOPUZKJSA-L 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000012792 core layer Substances 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011257 shell material Substances 0.000 description 1
- 230000028016 temperature homeostasis Effects 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 239000002918 waste heat Substances 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
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
-
- 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
- C09K5/02—Materials undergoing a change of physical state when used
-
- 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
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
-
- 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
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
-
- 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
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Combustion & Propulsion (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Multicomponent Fibers (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention relates to technical field of phase-change energy storage, the solid-solid phase change composite fibre being more particularly to crosslinked online with skin-core structure and sandwich layer and preparation method thereof.The composite fibre is using alginate as cortex, with allyl polyglycol, Triallyl isocyanurate and initiator are sandwich layer, the composite fibre with skin-core structure is obtained using wet spinning technology, and it is heat-treated during fiber post-processing, so that sandwich layer carries out cross-linking reaction, the solid-solid phase change material that there is sandwich layer to be cross-linked structure is obtained, cortex is the composite fibre of alginate.The stability of fiber is good, crystallization enthalpy is high and preparation method is simple, has a good application prospect.
Description
Technical field
It is more particularly to a kind of to be crosslinked online with skin-core structure and sandwich layer the present invention relates to technical field of phase-change energy storage
Solid-solid phase-change composite fibre and the composite fibre preparation method.
Background technology
Phase-change material (PCMs) refer to environment temperature drive under can store or discharge heat energy and its own temperature keep not
The functional material of change.In recent years application constantly expands PCMs, in Solar use, Waste Heat Recovery, agricultural greenhouse greenhouse, intelligence
The fields such as energy air-conditioning and construction, clothes insulation, the protection of electronic device constant temperature, energy storage cooker and camouflage have been applied.Generally
PCMs is difficult to directly using, it is necessary to by encapsulation, blending or the working process such as be modified to meet real requirement.Common pair
PCMs processing and treating methods mainly have：1. mechanical means, load using by phase-change material among a kind of container, definite shape is made
Heat-storage thermoregulation device, this method is used for inorganic phase-change material；2. physical method, phase-change material is mutually mixed with material of main part
Closing, material of main part is used as carrier, such as mixes certain nanometer or the textile fabric of micron order phase-change material preparation, or by phase transformation material
Material is blended with certain backing material, is compared the two and is firmly combined together, is prepared into shaping phase-change material or shape
Stable phase-change material；3. microcapsule method, it is prepared into as shell material micro- using phase-change material as core, some polymeric materials
Capsule, phase-change material is avoided directly to be touched with external environment；4. chemical method, under the premise of material phase transformation energy storage characteristic is kept, lead to
Cross chemical method to be modified, be transformed into new compound, it is met application requirement, phase-change material such as is connect into branch arrives polymer
On macromolecular chain, and phase-change material is subjected to crosslinking Treatment etc..
Using composite spinning technology, polymer and phase-change material melt or solution are directly spun into core-skin type phase change fiber
It is phase-change material and the perfect combining form of fibre-forming polymer.Zhang Xingxiang et al. is using polypropylene (PP) and molecular weight as 1000-
20000 polyethylene glycol (PEG) and thickener is primary raw material, and core-sheath is have developed using the method for melt composite spinning
Phase change fiber, the fiber process is into 490g/ ㎡ non-woven cloth, and at 35.5 DEG C or so, the purer polypropylene fibre of its internal temperature is non-woven
Cloth is low 3.3 DEG C, high 6.1 DEG C in 26.9 DEG C or so the purer polypropylene non-woven fabrics of its internal temperature.But compound fibre prepared by the method
The wrapped up sandwich layer of dimension is solid-liquid phase change material, can not be wrapped up solid-solid phase transition material.So fibre that this method obtains
Dimension still has the leakage problem of sandwich layer phase-change material.
The content of the invention
The present invention for solves the problems, such as the difficult processing of solid-solid phase-change fiber in the prior art, it is easy reveal, enthalpy of phase change is small provides
A kind of preparation method of the solid-solid phase-change composite fibre being crosslinked online with skin-core structure and sandwich layer and the composite fibre.With sea
Alginates are cortex, the phase transformation prepared with allyl polyglycol monomer, Triallyl isocyanurate crosslinking agent and initiator
Material is sandwich layer, and the composite fibre with skin-core structure is obtained using wet spinning technology, and right during fiber post-processing
It is heat-treated so that and sandwich layer carries out online cross-linking reaction, obtains the solid-solid phase transition material that there is sandwich layer to be cross-linked structure,
Cortex is the composite fibre of alginate.The composite fibre stability is good, crystallization enthalpy is high, and preparation method is simple, has good
Application prospect.
First purpose of the invention is that the compound fibre of solid-solid phase-change being crosslinked online with skin-core structure and sandwich layer is claimed
Dimension, using alginate as cortex, with the phase-change material of allyl polyglycol, Triallyl isocyanurate and initiator preparation
For sandwich layer, composite fibre is obtained.Alginate can be sodium alginate and/or calcium alginate.
Preferably, the mol ratio of the allyl polyglycol and Triallyl isocyanurate is 1：1~1:5；It is described
Initiator accounts for the 3~7% of Triallyl isocyanurate and allyl polyglycol gross mass.
Second purpose of the invention is that the compound fibre of solid-solid phase-change being crosslinked online with skin-core structure and sandwich layer is claimed
The preparation method of dimension, comprises the following steps：
(1) preparation of sandwich layer phase-change material：Allyl polyglycol is heated up to melt, adds triallyl isocyanuric acid
Ester and initiator, make it well mixed under high velocity agitation, obtain sandwich layer phase-change material melt；
(2) preparation of cortex spinning solution：After sodium alginate is made into sodium alginate soln with water, vacuum defoamation is carried out；
(3) preparation of composite fibre：Sandwich layer phase-change material melt is fitted into sandwich layer spinning box, sodium alginate soln loads
In cortex spinning box, sandwich layer melt and cortex solution enter composite spinneret, and fiber in coagulating bath is squeezed into through composite spinneret
Shaping, the fiber of shaping is heat-treated so that core material carries out online cross-linking reaction, obtains having skin-core structure
Solid-solid phase-change fiber.
Preferably, described allyl polyglycol molecular weight is 2400.
Preferably, described initiator is benzoyl peroxide or azodiisobutyronitrile.
Preferably, sodium alginate soln concentration is 3~5wt%
Preferably, the melting temperature described in step (1) is 65~80 DEG C.It is furthermore preferred that first allyl polyglycol is added
Temperature adds Triallyl isocyanurate and initiator is better to 70 DEG C of meltings.
Preferably, step (2) the vacuum defoamation time is 4~6h.
Preferably, the calcium chloride containing 3~5wt% in step (3) described coagulating bath.
Preferably, the heat treatment temperature described in step (3) is 100~130 DEG C, and heat treatment time is 60~100s.
By the way that the phase-change material melt of preparation is fitted into sandwich layer spinning box, sodium alginate soln loads cortex and spun the present invention
In silk tank, cortex and sandwich layer stoste enter composite spinneret, are squeezed into through spinneret in coagulating bath, the fiber in the presence of coagulating bath
Shaping, the fiber of shaping is heat-treated so that core material carries out online cross-linking reaction, is finally changed into solid-solid phase-change
Material, it is prepared for the solid-solid phase-change composite fibre that there is skin-core structure and sandwich layer to be crosslinked online.
Compared with prior art, the present invention has advantages below：
(1) present invention prepares the phase change fiber of skin-core structure using wet method composite spinning method, and alginate is cortex, phase transformation
Material allyl polyglycol, crosslinking agent and initiator are sandwich layer, and core material carries out cross-linking reaction during heat treatment, is prepared for one
The solid-solid phase-change composite fibre that kind is crosslinked with skin-core structure and sandwich layer, avoids phase-change material leakage problem；
(2) the phase change fiber crystallization enthalpy prepared by the present invention is 86.45~88.48J/g, crystallization temperature 34.56 DEG C~
Between 35.53 DEG C, have wide practical use in textile industry；
(3) present invention process is simple, and to composite spinning technology free of claims, and production cost is low, is easy to industrial metaplasia
Production.
Brief description of the drawings
Fig. 1 is the solid-solid phase-change composite fibre microphotograph that there is skin-core structure and sandwich layer to be crosslinked prepared by the present invention；
Fig. 2 is the DSC curve of composite fibre prepared by the embodiment of the present invention 1.
Embodiment
Below by specific embodiment, the present invention will be described in detail, but the embodiment is not used in the guarantor of the limitation present invention
Protect scope.Material therefor in following embodiments, reagent etc., unless otherwise specified, commercially obtain.
Embodiment 1
It is prepared by sandwich layer phase-change material：The allyl polyglycol that molecular weight is 2400 is warmed to 70 DEG C of meltings, add etc.
Mole Triallyl isocyanurate and ground mistake initiator B PO, BPO accounts for above-mentioned raw materials gross mass 3%, in high-speed stirring
Mixing down makes it well mixed.
The preparation of cortex sodium alginate spinning solution：Taking certain sodium alginate and water to be made into after 3% solution, to carry out 4h true
Empty deaeration.
The preparation of composite fibre：Phase-change material melt prepared by the above method is fitted into sandwich layer spinning box, sodium alginate
Solution is fitted into cortex spinning box, and cortex and sandwich layer stoste enter composite spinneret, is squeezed into through spinneret solidifying containing 3% calcium chloride
Gu in bath, the fiberizing in the presence of coagulating bath, the fiber of shaping is subjected to 80s heat treatments at 120 DEG C so that core material
Online cross-linking reaction is carried out, is finally changed into the solid-solid phase-change fiber of skin-core structure, its shape characteristic is as shown in Figure 1.Prepare
Phase change fiber crystallization break and crystallization temperature be respectively 88.48J/g, 35.53 DEG C.
DSC differential scanning calorimetric analysis are researched and analysed (as shown in Figure 2) shows not thermally treated core-skin composite fiber
Crystallization temperature is 33.90 DEG C, and the composite fibre crystallization temperature through above-mentioned condition heat treatment is 35.53 DEG C, crystallization temperature rise
1.63 DEG C, the mobility for indicating chain declines, and illustrates that there occurs cross-linking reaction in heat treatment process center core layer.
Embodiment 2
It is prepared by sandwich layer phase-change material：The allyl polyglycol that molecular weight is 2400 is warmed to 65 DEG C of meltings, addition rubs
You are than being 1:The initiator B PO for accounting for quality 4% of 2 Triallyl isocyanurate and ground mistake, makes under high velocity agitation
It is well mixed.
The preparation of cortex sodium alginate spinning solution：Taking certain sodium alginate and water to be made into after 4% solution, to carry out 5h true
Empty deaeration.
The preparation of composite fibre：Phase-change material melt prepared by the above method is fitted into sandwich layer spinning box, sodium alginate
Solution is fitted into cortex spinning box, and cortex and sandwich layer stoste enter composite spinneret, is squeezed into through spinneret solidifying containing 5% calcium chloride
Gu in bath, the fiberizing in the presence of coagulating bath, the fiber of shaping is subjected to 60s heat treatments at 100 DEG C so that core material
Cross-linking reaction is carried out, is finally changed into the solid-solid phase-change fiber of skin-core structure.The phase change fiber crystallization break and crystallization temperature of preparation
Respectively 87.51J/g, 35.10 DEG C
Embodiment 3
It is prepared by sandwich layer phase-change material：The allyl polyglycol that molecular weight is 2400 is warmed to 80 DEG C of meltings, addition rubs
You are than being 1:The initiator B PO for accounting for quality 5% of 3 Triallyl isocyanurate and ground mistake, makes under high velocity agitation
It is well mixed.
The preparation of cortex sodium alginate spinning solution：Taking certain sodium alginate and water to be made into after 5% solution, to carry out 6h true
Empty deaeration.
The preparation of composite fibre：Phase-change material melt prepared by the above method is fitted into sandwich layer spinning box, sodium alginate
Solution is fitted into cortex spinning box, and cortex and sandwich layer stoste enter composite spinneret, is squeezed into through spinneret solidifying containing 4% calcium chloride
Gu in bath, the fiberizing in the presence of coagulating bath, the fiber of shaping is subjected to 110S heat treatments at 120 DEG C so that sandwich layer material
Material carries out cross-linking reaction, is finally changed into the solid-solid phase-change fiber of skin-core structure.The phase change fiber crystallization break of preparation and crystallization temperature
It is respectively 87.90J/g to spend, 35.50 DEG C
Embodiment 4
It is prepared by sandwich layer phase-change material：The allyl polyglycol that molecular weight is 2400 is warmed to 70 DEG C of meltings, addition rubs
You are than being 1:The initiator B PO for accounting for quality 6% of 4 Triallyl isocyanurate and ground mistake, makes under high velocity agitation
It is well mixed.
The preparation of cortex sodium alginate spinning solution：Taking certain sodium alginate and water to be made into after 3% solution, to carry out 5h true
Empty deaeration.
The preparation of composite fibre：Phase-change material melt prepared by the above method is fitted into sandwich layer spinning box, sodium alginate
Solution is fitted into cortex spinning box, and cortex and sandwich layer stoste enter composite spinneret, is squeezed into through spinneret solidifying containing 5% calcium chloride
Gu in bath, the fiberizing in the presence of coagulating bath, the fiber of shaping is subjected to 70s heat treatments at 130 DEG C so that core material
Cross-linking reaction is carried out, is finally changed into the solid-solid phase-change fiber of skin-core structure.The phase change fiber crystallization break and crystallization temperature of preparation
Respectively 86.45J/g, 35.06 DEG C
Embodiment 5
It is prepared by sandwich layer phase-change material：The allyl polyglycol that molecular weight is 2400 is warmed to 70 DEG C of meltings, addition rubs
You are than being 1:The initiator B PO for accounting for quality 7% of 5 Triallyl isocyanurate and ground mistake, makes under high velocity agitation
It is well mixed.
The preparation of cortex sodium alginate spinning solution：Taking certain sodium alginate and water to be made into after 3% solution, to carry out 5h true
Empty deaeration.
The preparation of composite fibre：Phase-change material melt prepared by the above method is fitted into sandwich layer spinning box, sodium alginate
Solution is fitted into cortex spinning box, and cortex and sandwich layer stoste enter composite spinneret, is squeezed into through spinneret solidifying containing 5% calcium chloride
Gu in bath, the fiberizing in the presence of coagulating bath, the fiber of shaping is subjected to 60S heat treatments at 120 DEG C so that core material
Cross-linking reaction is carried out, is finally changed into the solid-solid phase-change fiber of skin-core structure.The phase change fiber crystallization break and crystallization temperature of preparation
Respectively 87.38J/g, 35.52 DEG C
Embodiment 6
It is prepared by sandwich layer phase-change material：The allyl polyglycol that molecular weight is 2400 is warmed to 70 DEG C of meltings, add etc.
Mole Triallyl isocyanurate and ground mistake the initiator A IBN for accounting for quality 3%, make it mixed under high velocity agitation
Close uniform.
The preparation of cortex sodium alginate spinning solution：Taking certain sodium alginate and water to be made into after 3% solution, to carry out 5h true
Empty deaeration.
The preparation of composite fibre：Phase-change material melt prepared by the above method is fitted into sandwich layer spinning box, sodium alginate
Solution is fitted into cortex spinning box, and cortex and sandwich layer stoste enter composite spinneret, is squeezed into through spinneret solidifying containing 5% calcium chloride
Gu in bath, the fiberizing in the presence of coagulating bath, the fiber of shaping is subjected to 100s heat treatments at 120 DEG C so that sandwich layer material
Material carries out cross-linking reaction, is finally changed into the solid-solid phase-change fiber of skin-core structure.The phase change fiber crystallization break of preparation and crystallization temperature
It is respectively 86.38J/g to spend, 34.95 DEG C
Embodiment 7
It is prepared by sandwich layer phase-change material：The allyl polyglycol that molecular weight is 2400 is warmed to 70 DEG C of meltings, add etc.
Mole Triallyl isocyanurate and ground mistake the initiator A IBN for accounting for quality 5%, make it mixed under high velocity agitation
Close uniform.
The preparation of cortex sodium alginate spinning solution：Taking certain sodium alginate and water to be made into after 3% solution, to carry out 5h true
Empty deaeration.
The preparation of composite fibre：Phase-change material melt prepared by the above method is fitted into sandwich layer spinning box, sodium alginate
Solution is fitted into cortex spinning box, and cortex and sandwich layer stoste enter composite spinneret, is squeezed into through spinneret solidifying containing 5% calcium chloride
Gu in bath, the fiberizing in the presence of coagulating bath, the fiber of shaping is subjected to 100S heat treatments at 120 DEG C so that sandwich layer material
Material carries out cross-linking reaction, is finally changed into the solid-solid phase-change fiber of skin-core structure.The phase change fiber crystallization break of preparation and crystallization temperature
It is respectively 80.33J/g to spend, 35.11 DEG C
Embodiment 8
It is prepared by sandwich layer phase-change material：The allyl polyglycol that molecular weight is 2400 is warmed to 70 DEG C of meltings, add etc.
Mole Triallyl isocyanurate and ground mistake the initiator B PO for accounting for quality 4%, make its mixing under high velocity agitation
Uniformly.
The preparation of cortex sodium alginate spinning solution：Taking certain sodium alginate and water to be made into after 3% solution, to carry out 5h true
Empty deaeration.
The preparation of composite fibre：Phase-change material melt prepared by the above method is fitted into sandwich layer spinning box, sodium alginate
Solution is fitted into cortex spinning box, and cortex and sandwich layer stoste enter composite spinneret, is squeezed into through spinneret solidifying containing 5% calcium chloride
Gu in bath, the fiberizing in the presence of coagulating bath, the fiber of shaping is subjected to 60s heat treatments at 100 DEG C so that core material
Cross-linking reaction is carried out, is finally changed into the solid-solid phase-change fiber of skin-core structure.The phase change fiber crystallization break and crystallization temperature of preparation
Respectively 85.31J/g, 33.95 DEG C
Embodiment 9
It is prepared by sandwich layer phase-change material：The allyl polyglycol that molecular weight is 2400 is warmed to 70 DEG C of meltings, add etc.
Mole Triallyl isocyanurate and ground mistake the initiator B PO for accounting for quality 4%, make its mixing under high velocity agitation
Uniformly.
The preparation of cortex sodium alginate spinning solution：Taking certain sodium alginate and water to be made into after 3% solution, to carry out 5h true
Empty deaeration.
The preparation of composite fibre：Phase-change material melt prepared by the above method is fitted into sandwich layer spinning box, sodium alginate
Solution is fitted into cortex spinning box, and cortex and sandwich layer stoste enter composite spinneret, is squeezed into through spinneret solidifying containing 5% calcium chloride
Gu in bath, the fiberizing in the presence of coagulating bath, the fiber of shaping is subjected to 100s heat treatments at 130 DEG C so that sandwich layer material
Material carries out cross-linking reaction, is finally changed into the solid-solid phase-change fiber of skin-core structure.The phase change fiber crystallization break of preparation and crystallization temperature
It is respectively 87.35J/g to spend, 35.51 DEG C.
Claims (9)
1. the solid-solid phase-change composite fibre being crosslinked online with skin-core structure and sandwich layer, it is characterised in that using alginate as skin
Layer, using the phase-change material of allyl polyglycol monomer, Triallyl isocyanurate crosslinking agent and initiator preparation as sandwich layer,
The composite fibre with skin-core structure is obtained using wet spinning technology, and hot place is carried out to it during fiber post-processing
Reason so that sandwich layer carries out online cross-linking reaction, obtains the solid-solid phase transition material that there is sandwich layer to be cross-linked structure, cortex is marine alga
The composite fibre of hydrochlorate；The mol ratio of the allyl polyglycol and Triallyl isocyanurate is 1：1~1：5；It is described
Initiator accounts for the 3~7% of Triallyl isocyanurate and allyl polyglycol gross mass.
A kind of 2. preparation of the solid-solid phase-change composite fibre being crosslinked online with skin-core structure and sandwich layer described in claim 1
Method, it is characterised in that comprise the following steps：
(1) preparation of sandwich layer phase-change material：Allyl polyglycol is heated up to melt, add Triallyl isocyanurate and
Initiator, make it well mixed under high velocity agitation, obtain sandwich layer phase-change material melt；
(2) preparation of cortex spinning solution：After sodium alginate is made into sodium alginate soln with water, vacuum defoamation is carried out；
(3) preparation of composite fibre：Sandwich layer phase-change material melt is fitted into sandwich layer spinning box, sodium alginate soln loads cortex
In spinning box, sandwich layer melt and cortex solution enter composite spinneret, and fiberizing in coagulating bath is squeezed into through composite spinneret,
The fiber of shaping is heat-treated so that core material carries out online cross-linking reaction, obtains the solid-solid phase with skin-core structure
Become fiber.
3. a kind of solid-solid phase-change composite fibre being crosslinked online with skin-core structure and sandwich layer according to claim 2
Preparation method, it is characterised in that described allyl polyglycol molecular weight is 2400.
4. a kind of solid-solid phase-change composite fibre being crosslinked online with skin-core structure and sandwich layer according to claim 2
Preparation method, it is characterised in that described initiator is benzoyl peroxide or azodiisobutyronitrile.
5. a kind of solid-solid phase-change composite fibre being crosslinked online with skin-core structure and sandwich layer according to claim 2
Preparation method, it is characterised in that sodium alginate soln concentration is 3~5wt%.
6. a kind of solid-solid phase-change composite fibre being crosslinked online with skin-core structure and sandwich layer according to claim 2
Preparation method, it is characterised in that the melting temperature described in step (1) is 65~80 DEG C.
7. a kind of solid-solid phase-change composite fibre being crosslinked online with skin-core structure and sandwich layer according to claim 2
Preparation method, it is characterised in that step (2) the vacuum defoamation time is 4~6h.
8. a kind of solid-solid phase-change composite fibre being crosslinked online with skin-core structure and sandwich layer according to claim 2
Preparation method, it is characterised in that the calcium chloride containing 3~5wt% in step (3) described coagulating bath.
9. a kind of solid-solid phase-change composite fibre being crosslinked online with skin-core structure and sandwich layer according to claim 2
Preparation method, it is characterised in that the heat treatment temperature described in step (3) is 100~130 DEG C, and heat treatment time is 60~100s.
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| CN111005086B (en) * | 2019-11-29 | 2022-05-27 | 吉祥三宝高科纺织有限公司 | Phase-change temperature-regulating fiber and preparation method thereof |
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| CN101787585A (en) * | 2001-09-21 | 2010-07-28 | 奥特拉斯技术有限公司 | Multi-component fibers having reversible thermal properties and methods of manufacturing thereof |
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