CN105648578A - Solid-solid phase-change composite fiber with skin-core structure and online cross-linked core layer and preparation method of solid-solid phase-change composite fiber - Google Patents
Solid-solid phase-change composite fiber with skin-core structure and online cross-linked core layer and preparation method of solid-solid phase-change composite fiber Download PDFInfo
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- CN105648578A CN105648578A CN201610012846.6A CN201610012846A CN105648578A CN 105648578 A CN105648578 A CN 105648578A CN 201610012846 A CN201610012846 A CN 201610012846A CN 105648578 A CN105648578 A CN 105648578A
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- 239000000835 fiber Substances 0.000 title claims abstract description 88
- 239000002131 composite material Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 51
- 239000007787 solid Substances 0.000 title claims abstract description 35
- 239000012792 core layer Substances 0.000 title abstract description 6
- 239000012782 phase change material Substances 0.000 claims abstract description 50
- 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 22
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 21
- 239000003999 initiator Substances 0.000 claims abstract description 21
- 238000004132 cross linking Methods 0.000 claims abstract description 19
- 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 8
- 229940072056 alginate Drugs 0.000 claims abstract description 8
- 235000010443 alginic acid Nutrition 0.000 claims abstract description 8
- 229920000615 alginic acid Polymers 0.000 claims abstract description 8
- 239000011162 core material Substances 0.000 claims description 45
- 238000009987 spinning Methods 0.000 claims description 39
- 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
- 230000001112 coagulating effect Effects 0.000 claims description 24
- 239000010695 polyglycol Substances 0.000 claims description 20
- 229920000151 polyglycol Polymers 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000000465 moulding Methods 0.000 claims description 12
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 11
- 238000013019 agitation Methods 0.000 claims description 11
- 239000001110 calcium chloride Substances 0.000 claims description 11
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 11
- 239000000155 melt Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 3
- 235000019400 benzoyl peroxide Nutrition 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
- 239000010410 layer Substances 0.000 abstract description 51
- 238000000034 method Methods 0.000 abstract description 24
- 230000008569 process Effects 0.000 abstract description 5
- 238000004146 energy storage Methods 0.000 abstract description 4
- 239000002202 Polyethylene glycol Substances 0.000 abstract description 3
- 229920001223 polyethylene glycol Polymers 0.000 abstract description 3
- 238000002166 wet spinning Methods 0.000 abstract description 2
- 238000012805 post-processing Methods 0.000 abstract 1
- 239000011232 storage material Substances 0.000 abstract 1
- 238000007669 thermal treatment Methods 0.000 abstract 1
- 238000002425 crystallisation Methods 0.000 description 24
- 230000008025 crystallization Effects 0.000 description 24
- 239000000243 solution Substances 0.000 description 21
- 230000008859 change Effects 0.000 description 15
- 239000012071 phase Substances 0.000 description 15
- 230000000694 effects Effects 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 239000011550 stock solution Substances 0.000 description 10
- 239000004743 Polypropylene Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000002135 phase contrast microscopy Methods 0.000 description 4
- 229920001155 polypropylene Polymers 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 3
- -1 polypropylene Polymers 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 239000003431 cross linking reagent Substances 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003094 microcapsule Substances 0.000 description 2
- 239000004745 nonwoven fabric Substances 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
- 238000004458 analytical method 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
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
- 238000010036 direct spinning Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000178 monomer 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
- 238000011160 research Methods 0.000 description 1
- 238000007493 shaping process 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
- 230000009466 transformation Effects 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 238000009941 weaving 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
- D01F8/18—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
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- 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)
- Multicomponent Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to the technical field of phase-change energy storage materials, and in particular relates to a solid-solid phase-change composite fiber with a skin-core structure and an online cross-linked core layer and a preparation method of the solid-solid phase-change composite fiber. With alginate as a skin layer, and allyl polyethylene glycol, triallyl isocyanurate and an initiator as a core layer, the composite fiber with the skin-core structure is obtained by a wet spinning technique, thermal treatment is carried out in the fiber post-processing process, and then the core layer is subjected to cross-linking reaction to obtain the composite fiber with the solid-solid phase-change material of the cross-linked structure as the core layer and the alginate as the skin layer. The fiber is good in stability, high in crystalline enthalpy and simple in preparation method and has a good application prospect.
Description
Technical field
The present invention relates to technical field of phase-change energy storage, there is skin-core structure and the preparation method of solid-solid phase-change composite fibre that sandwich layer cross-links online and this composite fibre particularly to a kind of.
Background technology
Phase-change material (PCMs) refers to can store or discharge heat energy and functional material that himself temperature remains unchanged under ambient temperature drives. PCMs range of application in recent years constantly expands, and is applied in fields such as Solar use, Waste Heat Recovery, agricultural greenhouse booth, intelligent air condition building, clothing insulation, the protection of electronic device constant temperature, energy storage cooker and camouflages. Usual PCMs is difficult to direct use, it is necessary to through encapsulation, the processed such as blended or modified to meet real requirement. Common mainly has PCMs processing and treating method: 1. mechanical means, adopts and is loaded in the middle of a kind of container by phase-change material, makes the heat-storage thermoregulation device of definite shape, and the method is used for mineral-type phase-change material; 2. physical method, phase-change material is mixed mutually with material of main part, material of main part is as carrier, such as textile fabric prepared by some kinds nanometer or micron order phase-change material, or phase-change material and certain backing material are carried out blended, make the two compare to be firmly combined together, prepare into the phase-change material of shaping phase-change material or dimensionally stable; 3. microcapsule method, using phase-change material as core, some polymeric material prepares into microcapsule as shell material, it is to avoid phase-change material and external environment are directly touched; 4. chemical method, under keeping material phase transformation energy storage characteristic premise, is modifiied by chemical method, it is transformed into new compound, make it meet application requirement, prop up to polymer macromolecule chain as phase-change material is connect, and phase-change material is carried out crosslinking Treatment etc.
Adopting composite spinning technology, it is phase-change material and the perfect combining form of fibre-forming polymer that polymer and phase-change material melt or solution Direct Spinning are made core-skin type phase change fiber. Zhang Xingxiang et al. with polypropylene (PP) and molecular weight be 1000-20000 Polyethylene Glycol (PEG) and thickening agent for primary raw material, the method adopting melt composite spinning have developed core-sheath phase change fiber, this fiber process becomes the non-weaving cloth of 490g/, when about 35.5 DEG C, the purer polypropylene non-woven fabric of its internal temperature is low 3.3 DEG C, high 6.1 DEG C at about the 26.9 DEG C purer polypropylene non-woven fabrics of its internal temperature.But the sandwich layer that composite fibre prepared by the method wraps up is solid-liquid phase change material, it is impossible to wrapped up by solid-solid phase transition material. So, the fiber that the method obtains yet suffers from the leakage problem of sandwich layer phase-change material.
Summary of the invention
The present invention solves the processing of solid-solid phase-change fiber difficulty in prior art, easily reveal, problem that enthalpy of phase change is little provides a kind of has a skin-core structure and the preparation method of solid-solid phase-change composite fibre that sandwich layer cross-links online and this composite fibre. With alginate for cortex, the phase-change material prepared with allyl polyglycol monomer, Triallyl isocyanurate cross-linking agent and initiator is for sandwich layer, wet spinning technology is adopted to obtain the composite fibre with skin-core structure, and in fiber post-treatment process, it is carried out heat treatment, sandwich layer is made to carry out online cross-linking reaction, obtaining having the solid-solid phase transition material that sandwich layer is cross-linked structure, cortex is the composite fibre of alginate. This composite fibre good stability, crystallization enthalpy are high, and preparation method is simple, has a good application prospect.
First purpose of the present invention is to be claimed to have a skin-core structure and solid-solid phase-change composite fibre that sandwich layer cross-links online; with alginate for cortex; the phase-change material prepared with allyl polyglycol, Triallyl isocyanurate and initiator, for sandwich layer, obtains composite fibre. Alginate can be sodium alginate and/or calcium alginate.
Preferably, described allyl polyglycol is 1:1��1:5 with the mol ratio of Triallyl isocyanurate; Described initiator accounts for the 3��7% of Triallyl isocyanurate and allyl polyglycol gross mass.
Second purpose of the present invention is to be claimed to have a skin-core structure and the preparation method of solid-solid phase-change composite fibre that sandwich layer cross-links online, comprises the following steps:
(1) preparation of sandwich layer phase-change material: allyl polyglycol is heated to melted, add Triallyl isocyanurate and initiator, make its mix homogeneously under high velocity agitation, obtain sandwich layer phase-change material melt;
(2) preparation of cortex spinning solution: sodium alginate and water carry out vacuum defoamation after being made into sodium alginate soln;
(3) preparation of composite fibre: sandwich layer phase-change material melt is loaded in sandwich layer spinning box, sodium alginate soln loads in cortex spinning box, sandwich layer melt and cortex solution enter composite spinneret, it is squeezed in coagulating bath fiberizing through composite spinneret, the fiber of molding is carried out heat treatment, make core material carry out online cross-linking reaction, obtain the solid-solid phase-change fiber with skin-core structure.
Preferably, described Triallyl isocyanurate molecular weight is 2400.
Preferably, described initiator is benzoyl peroxide or azodiisobutyronitrile.
Preferably, sodium alginate soln concentration is 3��5wt%
Preferably, the melt temperature described in step (1) is 65��80 DEG C. Melt it is furthermore preferred that first allyl polyglycol to be warmed to 70 DEG C, add Triallyl isocyanurate and initiator effect more preferably.
Preferably, step (2) the described vacuum defoamation time is 4��6h.
Preferably, containing 3��5wt% calcium chloride 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.
The present invention is by loading in sandwich layer spinning box by the phase-change material melt of preparation, sodium alginate soln loads in cortex spinning box, cortex and sandwich layer stock solution enter composite spinneret, clamp-on in coagulating bath through spinneret, fiberizing under the effect of coagulating bath, carries out heat treatment by the fiber of molding so that core material carries out online cross-linking reaction, finally it is changed into solid-solid phase transition material, is prepared for having skin-core structure and solid-solid phase-change composite fibre that sandwich layer cross-links online.
Compared with prior art, the invention have the advantages that
(1) present invention adopts wet method composite spinning method to prepare the phase change fiber of skin-core structure, alginate is cortex, phase-change material allyl polyglycol, cross-linking agent and initiator are sandwich layer, during heat treatment, core material carries out cross-linking reaction, it is prepared for a kind of solid-solid phase-change composite fibre with skin-core structure and sandwich layer crosslinking, it is to avoid phase-change material leakage problem;
(2) the phase change fiber crystallization enthalpy prepared by the present invention is 86.45��88.48J/g, and crystallization temperature, between 34.56 DEG C��35.53 DEG C, has 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, it is easy to industrialized production.
Accompanying drawing explanation
Fig. 1 be the present invention prepare have skin-core structure and sandwich layer crosslinking solid-solid phase-change composite fibre microphotograph;
Fig. 2 is the DSC curve of the composite fibre of the embodiment of the present invention 1 preparation.
Detailed description of the invention
Describe the present invention below by specific embodiment, but this embodiment is not used in and limits the scope of the invention. Material therefor in following embodiment, reagent etc., if no special instructions, all commercially obtain.
Embodiment 1
Prepared by sandwich layer phase-change material: the allyl polyglycol that molecular weight is 2400 is warmed to 70 DEG C and melts, add the initiator B PO of equimolar Triallyl isocyanurate and ground mistake, BPO accounts for above-mentioned raw materials gross mass 3%, makes its mix homogeneously under high velocity agitation.
The preparation of cortex sodium alginate spinning solution: take after certain sodium alginate is made into 3% solution with water and carry out 4h vacuum defoamation.
The preparation of composite fibre: the phase-change material melt prepared by said method loads in sandwich layer spinning box, sodium alginate soln loads in cortex spinning box, cortex and sandwich layer stock solution enter composite spinneret, in the coagulating bath containing 3% calcium chloride clamp-oned by spinneret, fiberizing under the effect of coagulating bath, carries out 80s heat treatment by the fiber of molding at 120 DEG C so that core material carries out online cross-linking reaction, finally being changed into the solid-solid phase-change fiber of skin-core structure, its shape characteristic is as shown in Figure 1. The phase change fiber crystallization break of preparation and crystallization temperature respectively 88.48J/g, 35.53 DEG C.
It is 33.90 DEG C without heat treated core-skin composite fiber crystallization temperature that DSC differential scanning calorimetric analysis (as shown in Figure 2) researchs and analyses display, it it is 35.53 DEG C through the heat treated composite fibre crystallization temperature of above-mentioned condition, crystallization temperature raises 1.63 DEG C, the mobility indicating chain declines, and describes and there occurs cross-linking reaction in heat treatment process center core layer.
Embodiment 2
Prepared by sandwich layer phase-change material: the allyl polyglycol that molecular weight is 2400 is warmed to 65 DEG C and melts, and adds the initiator B PO accounting for quality 4% that mol ratio is the Triallyl isocyanurate of 1:2 and ground mistake, makes its mix homogeneously under high velocity agitation.
The preparation of cortex sodium alginate spinning solution: take after certain sodium alginate is made into 4% solution with water and carry out 5h vacuum defoamation.
The preparation of composite fibre: the phase-change material melt prepared by said method loads in sandwich layer spinning box, sodium alginate soln loads in cortex spinning box, cortex and sandwich layer stock solution enter composite spinneret, in the coagulating bath containing 5% calcium chloride clamp-oned by spinneret, fiberizing under the effect of coagulating bath, the fiber of molding is carried out 60s heat treatment at 100 DEG C so that core material carries out cross-linking reaction, be finally changed into the solid-solid phase-change fiber of skin-core structure.The phase change fiber crystallization break of preparation and crystallization temperature respectively 87.51J/g, 35.10 DEG C
Embodiment 3
Prepared by sandwich layer phase-change material: the allyl polyglycol that molecular weight is 2400 is warmed to 80 DEG C and melts, and adds the initiator B PO accounting for quality 5% that mol ratio is the Triallyl isocyanurate of 1:3 and ground mistake, makes its mix homogeneously under high velocity agitation.
The preparation of cortex sodium alginate spinning solution: take after certain sodium alginate is made into 5% solution with water and carry out 6h vacuum defoamation.
The preparation of composite fibre: the phase-change material melt prepared by said method loads in sandwich layer spinning box, sodium alginate soln loads in cortex spinning box, cortex and sandwich layer stock solution enter composite spinneret, in the coagulating bath containing 4% calcium chloride clamp-oned by spinneret, fiberizing under the effect of coagulating bath, the fiber of molding is carried out 110S heat treatment at 120 DEG C so that core material carries out cross-linking reaction, be finally changed into the solid-solid phase-change fiber of skin-core structure. The phase change fiber crystallization break of preparation and crystallization temperature respectively 87.90J/g, 35.50 DEG C
Embodiment 4
Prepared by sandwich layer phase-change material: the allyl polyglycol that molecular weight is 2400 is warmed to 70 DEG C and melts, and adds the initiator B PO accounting for quality 6% that mol ratio is the Triallyl isocyanurate of 1:4 and ground mistake, makes its mix homogeneously under high velocity agitation.
The preparation of cortex sodium alginate spinning solution: take after certain sodium alginate is made into 3% solution with water and carry out 5h vacuum defoamation.
The preparation of composite fibre: the phase-change material melt prepared by said method loads in sandwich layer spinning box, sodium alginate soln loads in cortex spinning box, cortex and sandwich layer stock solution enter composite spinneret, in the coagulating bath containing 5% calcium chloride clamp-oned by spinneret, fiberizing under the effect of coagulating bath, the fiber of molding is carried out 70s heat treatment at 130 DEG C so that core material carries out cross-linking reaction, be finally changed into the solid-solid phase-change fiber of skin-core structure. The phase change fiber crystallization break of preparation and crystallization temperature respectively 86.45J/g, 35.06 DEG C
Embodiment 5
Prepared by sandwich layer phase-change material: the allyl polyglycol that molecular weight is 2400 is warmed to 70 DEG C and melts, and adds the initiator B PO accounting for quality 7% that mol ratio is the Triallyl isocyanurate of 1:5 and ground mistake, makes its mix homogeneously under high velocity agitation.
The preparation of cortex sodium alginate spinning solution: take after certain sodium alginate is made into 3% solution with water and carry out 5h vacuum defoamation.
The preparation of composite fibre: the phase-change material melt prepared by said method loads in sandwich layer spinning box, sodium alginate soln loads in cortex spinning box, cortex and sandwich layer stock solution enter composite spinneret, in the coagulating bath containing 5% calcium chloride clamp-oned by spinneret, fiberizing under the effect of coagulating bath, the fiber of molding is carried out 60S heat treatment at 120 DEG C so that core material carries out cross-linking reaction, be finally changed into the solid-solid phase-change fiber of skin-core structure. The phase change fiber crystallization break of preparation and crystallization temperature respectively 87.38J/g, 35.52 DEG C
Embodiment 6
Prepared by sandwich layer phase-change material: the allyl polyglycol that molecular weight is 2400 is warmed to 70 DEG C and melts, add the initiator A IBN accounting for quality 3% of equimolar Triallyl isocyanurate and ground mistake, make its mix homogeneously under high velocity agitation.
The preparation of cortex sodium alginate spinning solution: take after certain sodium alginate is made into 3% solution with water and carry out 5h vacuum defoamation.
The preparation of composite fibre: the phase-change material melt prepared by said method loads in sandwich layer spinning box, sodium alginate soln loads in cortex spinning box, cortex and sandwich layer stock solution enter composite spinneret, in the coagulating bath containing 5% calcium chloride clamp-oned by spinneret, fiberizing under the effect of coagulating bath, the fiber of molding is carried out 100s heat treatment at 120 DEG C so that core material carries out cross-linking reaction, be finally changed into the solid-solid phase-change fiber of skin-core structure. The phase change fiber crystallization break of preparation and crystallization temperature respectively 86.38J/g, 34.95 DEG C
Embodiment 7
Prepared by sandwich layer phase-change material: the allyl polyglycol that molecular weight is 2400 is warmed to 70 DEG C and melts, add the initiator A IBN accounting for quality 5% of equimolar Triallyl isocyanurate and ground mistake, make its mix homogeneously under high velocity agitation.
The preparation of cortex sodium alginate spinning solution: take after certain sodium alginate is made into 3% solution with water and carry out 5h vacuum defoamation.
The preparation of composite fibre: the phase-change material melt prepared by said method loads in sandwich layer spinning box, sodium alginate soln loads in cortex spinning box, cortex and sandwich layer stock solution enter composite spinneret, in the coagulating bath containing 5% calcium chloride clamp-oned by spinneret, fiberizing under the effect of coagulating bath, the fiber of molding is carried out 100S heat treatment at 120 DEG C so that core material carries out cross-linking reaction, be finally changed into the solid-solid phase-change fiber of skin-core structure. The phase change fiber crystallization break of preparation and crystallization temperature respectively 80.33J/g, 35.11 DEG C
Embodiment 8
Prepared by sandwich layer phase-change material: the allyl polyglycol that molecular weight is 2400 is warmed to 70 DEG C and melts, add the initiator B PO accounting for quality 4% of equimolar Triallyl isocyanurate and ground mistake, make its mix homogeneously under high velocity agitation.
The preparation of cortex sodium alginate spinning solution: take after certain sodium alginate is made into 3% solution with water and carry out 5h vacuum defoamation.
The preparation of composite fibre: the phase-change material melt prepared by said method loads in sandwich layer spinning box, sodium alginate soln loads in cortex spinning box, cortex and sandwich layer stock solution enter composite spinneret, in the coagulating bath containing 5% calcium chloride clamp-oned by spinneret, fiberizing under the effect of coagulating bath, the fiber of molding is carried out 60s heat treatment at 100 DEG C so that core material carries out cross-linking reaction, be finally changed into the solid-solid phase-change fiber of skin-core structure. The phase change fiber crystallization break of preparation and crystallization temperature respectively 85.31J/g, 33.95 DEG C
Embodiment 9
Prepared by sandwich layer phase-change material: the allyl polyglycol that molecular weight is 2400 is warmed to 70 DEG C and melts, add the initiator B PO accounting for quality 4% of equimolar Triallyl isocyanurate and ground mistake, make its mix homogeneously under high velocity agitation.
The preparation of cortex sodium alginate spinning solution: take after certain sodium alginate is made into 3% solution with water and carry out 5h vacuum defoamation.
The preparation of composite fibre: the phase-change material melt prepared by said method loads in sandwich layer spinning box, sodium alginate soln loads in cortex spinning box, cortex and sandwich layer stock solution enter composite spinneret, in the coagulating bath containing 5% calcium chloride clamp-oned by spinneret, fiberizing under the effect of coagulating bath, the fiber of molding is carried out 100s heat treatment at 130 DEG C so that core material carries out cross-linking reaction, be finally changed into the solid-solid phase-change fiber of skin-core structure. The phase change fiber crystallization break of preparation and crystallization temperature respectively 87.35J/g, 35.51 DEG C.
Claims (10)
1. having a skin-core structure and solid-solid phase-change composite fibre that sandwich layer cross-links online, it is characterised in that with alginate for cortex, the phase-change material prepared with allyl polyglycol, Triallyl isocyanurate and initiator, for sandwich layer, obtains composite fibre.
2. according to claim 1 have a skin-core structure and solid-solid phase-change composite fibre that sandwich layer cross-links online, it is characterised in that the mol ratio of described allyl polyglycol and Triallyl isocyanurate is 1:1��1:5; Described initiator accounts for the 3��7% of Triallyl isocyanurate and allyl polyglycol gross mass.
3. there is skin-core structure and the preparation method of solid-solid phase-change composite fibre that sandwich layer cross-links online described in a claim 1, it is characterised in that comprise the following steps:
(1) preparation of sandwich layer phase-change material: allyl polyglycol is heated to melted, add Triallyl isocyanurate and initiator, make its mix homogeneously under high velocity agitation, obtain sandwich layer phase-change material melt;
(2) preparation of cortex spinning solution: sodium alginate and water carry out vacuum defoamation after being made into sodium alginate soln;
(3) preparation of composite fibre: sandwich layer phase-change material melt is loaded in sandwich layer spinning box, sodium alginate soln loads in cortex spinning box, sandwich layer melt and cortex solution enter composite spinneret, it is squeezed in coagulating bath fiberizing through composite spinneret, the fiber of molding is carried out heat treatment, make core material carry out online cross-linking reaction, obtain the solid-solid phase-change fiber with skin-core structure.
4. according to claim 3 a kind of have a skin-core structure and the preparation method of solid-solid phase-change composite fibre that sandwich layer cross-links online, it is characterised in that described Triallyl isocyanurate molecular weight is 2400.
5. according to claim 3 a kind of have a skin-core structure and the preparation method of solid-solid phase-change composite fibre that sandwich layer cross-links online, it is characterised in that described initiator is benzoyl peroxide or azodiisobutyronitrile.
6. according to claim 3 a kind of have a skin-core structure and the preparation method of solid-solid phase-change composite fibre that sandwich layer cross-links online, it is characterised in that sodium alginate soln concentration is 3��5wt%.
7. according to claim 3 a kind of have a skin-core structure and the preparation method of solid-solid phase-change composite fibre that sandwich layer cross-links online, it is characterised in that the melt temperature described in step (1) is 65��80 DEG C.
8. according to claim 3 a kind of have a skin-core structure and the preparation method of solid-solid phase-change composite fibre that sandwich layer cross-links online, it is characterised in that step (2) the described vacuum defoamation time is 4��6h.
9. according to claim 3 a kind of have a skin-core structure and the preparation method of solid-solid phase-change composite fibre that sandwich layer cross-links online, it is characterised in that containing 3��5wt% calcium chloride in step (3) described coagulating bath.
10. according to claim 3 a kind of have a skin-core structure and the preparation method of solid-solid phase-change composite fibre that sandwich layer cross-links online, it is characterized in that, heat treatment temperature described in step (3) is 100��130 DEG C, and heat treatment time is 60��100s.
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