CN105369380B - Phase-change temperature-regulating cellulose fiber prepared by solvent method and preparation method thereof - Google Patents
Phase-change temperature-regulating cellulose fiber prepared by solvent method and preparation method thereof Download PDFInfo
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- CN105369380B CN105369380B CN201510911769.3A CN201510911769A CN105369380B CN 105369380 B CN105369380 B CN 105369380B CN 201510911769 A CN201510911769 A CN 201510911769A CN 105369380 B CN105369380 B CN 105369380B
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- 238000000034 method Methods 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 45
- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 33
- 239000002904 solvent Substances 0.000 title claims abstract description 21
- 238000009987 spinning Methods 0.000 claims abstract description 47
- 239000012782 phase change material Substances 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 35
- 230000008569 process Effects 0.000 claims abstract description 33
- 238000002156 mixing Methods 0.000 claims abstract description 31
- 239000000835 fiber Substances 0.000 claims abstract description 29
- 238000010521 absorption reaction Methods 0.000 claims abstract description 23
- 239000011148 porous material Substances 0.000 claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 12
- 238000001179 sorption measurement Methods 0.000 claims abstract description 11
- 239000002608 ionic liquid Substances 0.000 claims description 52
- 229920002678 cellulose Polymers 0.000 claims description 34
- 239000001913 cellulose Substances 0.000 claims description 34
- 238000001125 extrusion Methods 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 29
- 239000002202 Polyethylene glycol Substances 0.000 claims description 25
- 150000001875 compounds Chemical class 0.000 claims description 25
- 238000002844 melting Methods 0.000 claims description 19
- 230000008018 melting Effects 0.000 claims description 19
- 229920001223 polyethylene glycol Polymers 0.000 claims description 18
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 12
- 230000009466 transformation Effects 0.000 claims description 12
- -1 stearic acid compound Chemical class 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 230000008961 swelling Effects 0.000 claims description 8
- 235000021355 Stearic acid Nutrition 0.000 claims description 7
- 230000001112 coagulating effect Effects 0.000 claims description 7
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 7
- 239000008117 stearic acid Substances 0.000 claims description 7
- 229910052604 silicate mineral Inorganic materials 0.000 claims description 5
- 239000004575 stone Substances 0.000 claims description 5
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 4
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 4
- 241001330002 Bambuseae Species 0.000 claims description 4
- 229920000858 Cyclodextrin Polymers 0.000 claims description 4
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 4
- 229910021536 Zeolite Inorganic materials 0.000 claims description 4
- 239000011425 bamboo Substances 0.000 claims description 4
- 239000003610 charcoal Substances 0.000 claims description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 4
- 229910021389 graphene Inorganic materials 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- 239000010457 zeolite Substances 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000002808 molecular sieve Substances 0.000 claims description 3
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052613 tourmaline Inorganic materials 0.000 claims description 3
- 239000011032 tourmaline Substances 0.000 claims description 3
- 229940070527 tourmaline Drugs 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 14
- 239000000126 substance Substances 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract 3
- 238000002425 crystallisation Methods 0.000 abstract 1
- 230000008025 crystallization Effects 0.000 abstract 1
- 230000004927 fusion Effects 0.000 abstract 1
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 20
- 229920000297 Rayon Polymers 0.000 description 8
- 150000001450 anions Chemical class 0.000 description 8
- 150000001768 cations Chemical class 0.000 description 8
- 239000000155 melt Substances 0.000 description 8
- 230000018044 dehydration Effects 0.000 description 7
- 238000006297 dehydration reaction Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 239000004753 textile Substances 0.000 description 7
- 229920000151 polyglycol Polymers 0.000 description 6
- 239000010695 polyglycol Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 239000003094 microcapsule Substances 0.000 description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 3
- 239000003317 industrial substance Substances 0.000 description 3
- 229920000875 Dissolving pulp Polymers 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- 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
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention discloses a phase-change temperature-regulating cellulose fiber prepared by a solvent method, which comprises a porous material, a high-molecular phase-change material and a substance with a far infrared absorption function, wherein the mass ratio of the porous adsorption material to the substance with the far infrared absorption function to the high-molecular phase-change material is as follows: 1-30: 1-50: 10-100; the fusion enthalpy value of the fiber is more than or equal to 5.5J/g, and the crystallization enthalpy value is more than or equal to 5.3J/g. The preparation method of the fiber comprises the preparation steps of the composite polymer phase-change porous material; preparing a spinning solution; and (4) spinning. The preparation of the composite polymer phase-change porous material is completed by adding a porous adsorption material and a substance with far infrared absorption function into the melted polymer phase-change material for adsorption and blending. The phase-change temperature-regulating cellulose fiber prepared by the method has the characteristics of no pollution in production process and green and environment-friendly product, and meanwhile, the porous adsorption material is used for adsorbing the high-molecular phase-change material, so that the loss in the forming process is reduced, and the phase-change temperature-regulating function of the fiber is ensured.
Description
Technical field
The present invention relates to a kind of phase-changing and temperature-regulating cellulose fibre and preparation method thereof, specifically, is related to one kind with fiber
Plain pulp and composite phase-change material are raw material, and ionic liquid is phase-changing and temperature-regulating cellulose fibre and its method prepared by solvent, is belonged to
In textile technology field.
Technical background
Ionic liquid have the characteristics that steam force down, stable performance, non-volatile, favorable solubility, be widely used in organic
The fields such as synthesis, electrochemistry, materials chemistry, there is research and application prospect well.Cellulose is as environment-friendly simultaneously
Renewable resource receives much concern.In recent years, preparing cellulose fibre as solvent dissolving cellulose using ionic liquid turns into the field
One of emphasis direction of research.
As the improvement of people's living standards, chemical fibre industry gradually develops to functionalization, intelligent direction, mutually modify tone
Warm fiber is wherein important one kind.Phase-changing and temperature-regulating fiber is to be discharged or absorbed using phase-change material to dive in phase transition process
Heat, so as to have two-way automatic temperature-adjusting function.America and Europe etc. country pay attention to its research and development, output in domestic is relatively low, product based on import,
Hold at high price.
It is the main method for preparing phase-changing and temperature-regulating cellulose fibre using microcapsules technology, solution spinning processes, at present
Through successfully realize cellulose fibre be mainly viscose rayon phase-changing and temperature-regulating be modified, as Chinese patent ZL200610157441.8,
ZL200710014607.5、ZL200710123411.X、ZL201010164832.9、ZL 201010295055.1、ZL
201210357126.5,201310420382.9,201410616024.X etc. disclose the research of viscose rayon temperature adjustment modification.
But in the prior art because microcapsules synthesis technique is complicated, the reaction between solvent and auxiliary agent, cause phase change fiber cost height, function
Property is undesirable, and the flow of wet spinning technology is longer, efficiency is low, simultaneously because in production process of viscose fiber, uses
It is seriously polluted to industrial chemicals such as sodium hydroxide, carbon disulfide and sulfuric acid, and fiber formation process and subsequently arrange process
In, phase-change material is lost in serious, the problems such as energy absorption conversion ratio is not high, so, invent that a kind of production procedure is pollution-free, production
Thing is green and the preferable New-type phase change temperature-regulating fiber of feature turns into urgent problem during we research and develop.
Using ionic liquid as the solvent of cellulose, it is not required to activate when dissolving cellulose, and ionic liquid is easily recycled, can
Recycle, while be easy to auxiliary agent etc. to add using the system, and influence of the ionic liquid to auxiliary agent is smaller, this is cellulose fiber
The new varieties of dimension open a Tiao Xin roads, while also solve very well and carry out cellulose CSP institute using viscose process
The problem of running into.
The content of the invention
The phase-changing and temperature-regulating cellulose fibre and its system prepared in view of the deficiencies of the prior art, the present invention provides a kind of solvent method
Preparation Method, realize following goal of the invention：
（1）The phase-changing and temperature-regulating cellulose fibre that the present invention obtains is to far red light, it is seen that light has absorption so that the phase transformation
Temperature-regulating fiber has preferable feature, and the fibers melt enthalpy >=5.5J/g prepared, crystallizes enthalpy >=5.3J/g, and weaving adds
Work performance is good；
（2）Polymeric phase change material is adsorbed using porous adsorbing material, reduces the loss in its forming process,
The phase-changing and temperature-regulating function of fiber is ensure that, and combines the material with Far-infrared Absorption function, adds the absorption to light energy
And transformation efficiency；
（3）Using ionic liquid as the solvent of cellulose, spinning solution is prepared using double screw extruder high-temperature digestion, and
With reference to single screw extrusion machine, the melting effect of cellulose is improved, while realizes cellulose melting, dehydration, vacuum defoamation, phase
Shorten the time more than 90% for viscose process；
（4）Preparation method of the present invention, production procedure is short and abandons the complicated synthesis technique of microcapsules, and cost is notable
Reduce, production efficiency is high.
（5）Compared with viscose process technique, reduce the use of industrial chemicals, realize whole green non-pollution, reduce fibre
Tie up the environmental hazard of production process, and the harm to operating personnel.
（6）The fiber can particularly be cured extensively using clothes, bedding, medical supplies and non-woven material field
Treatment field, because raw material, production procedure, product green non-pollution, especially there is wide development space in medical field.
The technical scheme that the present invention takes is as follows：
Phase-changing and temperature-regulating cellulose fibre prepared by a kind of solvent method, the fiber include porous adsorbing material, macromolecule phase
Become material and the material with Far-infrared Absorption function.
The mass ratio of the porous adsorbing material, the material with Far-infrared Absorption function and polymeric phase change material three
For：1~30:1~50:10~100.
Fibers melt enthalpy >=the 5.5J/g, crystallize enthalpy >=5.3J/g.
The porous adsorbing material be expanded graphite, cyclodextrin, zeolite, molecular sieve, one kind in silicate mineral or
Person is several；Described silicate mineral is the one or more of montmorillonite, diatomite and kaolin soil.
The material with Far-infrared Absorption function is in graphene, tourmaline, medical stone, bamboo charcoal and carborundum
It is one or more of；The polymeric phase change material is that polyethylene glycol, polyethylene glycol acrylate, PEO/stearic acid are multiple
One or more in compound.
A kind of method that solvent method prepares phase-changing and temperature-regulating cellulose fibre, include the system of composite high-molecular phase transformation porous material
Standby step；The preparation process of spinning solution；Spinning process.
The preparation of the composite high-molecular phase transformation porous material is by porous adsorbing material, has Far-infrared Absorption function
Material is added to absorption blending in the polymeric phase change material that melting is completed and completed.
Described polymeric phase change material melting temperature and blending temperature are 60~100 °C.
The blending adsorption time is 1.0~4.0h.
The preparation process of the spinning solution includes blending step, swelling step, melt-off process.
In the blending step, the composite high-molecular phase transformation porous material for preparing completion is added into alkyl imidazole type ionic liquid
Body, cation are pi-allyl, ethyl, the one or more of butyl；Anion is halogen, SCN-And CH3COO-In one kind or
Person is a variety of, the ionic liquid after being blended.
The swelling step is that the ionic liquid after blending and the cellulose pulp after crushing are carried out into premixing swelling, is obtained
To blending ionic liquid and cellulose pulp compound.
Described blending ionic liquid and composite high-molecular phase transformation porous material in cellulose pulp compound：Cellulose slurry
The dregs of rice：The mass ratio of ionic liquid three is 1~6:15~30:64~84.
The melt-off process needs successively to pass through double screw extruder and single screw extrusion machine.
Each section of temperature is 80 ~ 150 DEG C in the double screw extruder, and screw speed is 50 ~ 200 revs/min, vacuum
For -0.05 ~ -0.10Mpa, each section of temperature range is 110 ~ 150 DEG C in the single screw extrusion machine, and screw speed is 50 ~ 120
Rev/min, vacuum is -0.05 ~ -0.10MPa, and Screw Extrusion pressure is 0.50 ~ 1.0 MPa.
In the spinning process, coagulating bath is the distilled water of 30~50 DEG C of temperature, or is concentration≤20%, temperature 30~
The aqueous solution of 50 DEG C of ionic liquid used.
Described porous adsorbing material, the material with Far-infrared Absorption function and the quality of polymeric phase change material three
Than for：1~30:1~50:10~100.
In process of production, can the needs according to production and the requirement to product, preparation technology to spinning solution, spin
Silk technique and aftertreatment technology carry out appropriate adjustment.
The present invention provides a kind of method that spinning technique using ionic liquid as solvent prepares phase-changing and temperature-regulating cellulose fibre,
Phase-changing and temperature-regulating cellulose fibre prepared by this method is based on the basis of polymeric phase change material, using porous material by high score
Sub- phase-change material melt absorption, and the material with Far-infrared Absorption function is combined, prepare the porous material of composite high-molecular phase transformation
Material, the composite high-molecular phase transformation porous material of above-mentioned preparation and ionic liquid are blended, and by cellulose pulp and above-mentioned blending
Liquid is mixed, and uses screw extrusion method to obtain the spinning solution using ionic liquid as solvent, and Gao Han is prepared using solvent spinning technique
The energy-saving and temperature-regulating cellulose fibre of value, there is the characteristics of production procedure is pollution-free, product is green.
The present invention uses the beneficial effect of above-mentioned technical proposal：
（1）The phase-changing and temperature-regulating cellulose fibre that the present invention obtains is to far red light, it is seen that light has absorption, the fiber of preparation
Enthalpy >=5.5J/g is melted, crystallizes enthalpy >=5.3J/g, textile process performance is good；
（2）Polymeric phase change material is adsorbed using porous adsorbing material, reduces the loss in its forming process,
The phase-changing and temperature-regulating function of fiber is ensure that, and combines the material with Far-infrared Absorption function, adds the absorption to light energy
And transformation efficiency；
（3）Using ionic liquid as the solvent of cellulose, spinning solution is prepared using double screw extruder high-temperature digestion, and
With reference to single screw extrusion machine, the melting effect of cellulose is improved, while realizes cellulose melting, dehydration, vacuum defoamation, with
Viscose process is compared to the shortening time 90%；
（4）Preparation method of the present invention, production procedure is short and abandons the complicated synthesis technique of microcapsules, and cost is notable
Reduce, technological process is short, production efficiency is high.
（5）Compared with viscose process technique, reduce the use of industrial chemicals, realize whole green non-pollution, reduce fibre
Tie up the environmental hazard of production process, and the harm to operating personnel.
With reference to embodiment, the present invention is described in detail.
Embodiment
The preferred embodiments of the present invention are illustrated below, it will be appreciated that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Content percentage in embodiment is mass percent.
Embodiment 1：
A kind of method that energy-saving and temperature-regulating cellulose fibre is prepared using ionic liquid as solvent, its key step include：
（1）The preparation of compound polyglycol porous phase-change material
Polyethylene glycol is melted at 60 DEG C, melts and silicate mineral-montmorillonite, electrically is added in the backward melt
Stone, the mass ratio for making silicate mineral, tourmaline and polyethylene glycol three are 1:1:10, blending adsorption time is 1.0h；
（2）The preparation of spinning solution
A, it is blended：Be pi-allyl by the compound polyglycol porous phase-change material of above-mentioned preparation and cation, anion be
The alkyl imidazole type ionic liquid of halogen is blended；
B, it is swelled：Ionic liquid after blending and the cellulose pulp after crushing are subjected to premixing swelling in proportion, its
In compound polyglycol porous phase-change material in obtained pre-mixed material：Cellulose pulp：The mass ratio of ionic liquid three
For 1:15: 84；
C, melt-off：Blending ionic liquid/cellulose pulp compound of preparation is added to twin-screw by charge door and squeezed
Go out machine, the temperature of double screw extruder is 80 DEG C, and screw speed is 200 revs/min, and vacuum is -0.05MPa, real in this process
Dehydration, deaeration and heating melting are showed；
The spinning solution of above-mentioned preparation is passed through into single screw extrusion machine, the temperature of single screw extrusion machine is 110 DEG C, and screw rod turns
Speed is 120 revs/min, and vacuum is -0.05MPa, spinning solution is further dehydrated, deaeration and mixed melting, Single screw extrusion
Pressure is 0.50MPa.
（3）Spinning
It it is 35 DEG C in temperature by spinning solution by measuring pump, spinneret in the case where Single screw extrusion pressure is 0.50MPa
Spinning moulding in distilled water coagulating bath, through drafting process, wash and the process that oils, the cellulose with phase-changing and temperature-regulating effect is made
Fiber.
Phase-changing and temperature-regulating cellulose fibre fiber made from embodiment 1 has good phase-changing and temperature-regulating function, melting enthalpy 5.5J/
G, enthalpy 5.3J/g is crystallized, textile process performance is good, and wearability is excellent.
Embodiment 2：
A kind of method that energy-saving and temperature-regulating cellulose fibre is prepared using ionic liquid as solvent, its key step include：
（1）The preparation of compound polyglycol porous phase-change material
Polyethylene glycol is melted at 70 DEG C, melts in the backward melt and adds zeolite, graphene, make zeolite, graphene
Mass ratio with polyethylene glycol three is 1:2:20, blending adsorption time is 2.0h；
（2）The preparation of spinning solution
A, it is blended：Be ethyl by the compound polyglycol porous phase-change material of above-mentioned preparation and cation, anion be
CH3COO-Alkyl imidazole type ionic liquid be blended；
B, it is swelled：By the ionic liquid after blending and the cellulose pulp after crushing by premixing swelling is carried out, wherein obtaining
To pre-mixed material in compound polyglycol porous phase-change material：Cellulose pulp：The mass ratio of ionic liquid three is 2:
20:78；
C, melt-off：Blending ionic liquid/cellulose pulp compound of preparation is added to twin-screw by charge door and squeezed
Go out machine, the temperature of double screw extruder is 89 DEG C, and screw speed is 176 revs/min, and vacuum is -0.06MPa, real in this process
Dehydration, deaeration and heating melting are showed；
The spinning solution of above-mentioned preparation is passed through into single screw extrusion machine, the temperature of single screw extrusion machine is 118 DEG C, and screw rod turns
Speed is 112 revs/min, and vacuum is -0.06MPa, spinning solution is further dehydrated, deaeration and mixed melting, Screw Extrusion pressure
Power is 0.57MPa.
（3）Spinning
In the case where Screw Extrusion pressure is 0.57MPa, spinning solution passes through measuring pump, spinneret, is 20% in concentration, temperature
Cation for 31 DEG C is ethyl, anion CH3COO-Alkyl imidazole type ionic liquid coagulating bath in spinning moulding, through leading
Stretch process, wash and the process that oils, the cellulose fibre with phase-changing and temperature-regulating effect is made.
Phase-changing and temperature-regulating cellulose fibre fiber made from embodiment 2 has good phase-changing and temperature-regulating function, melts enthalpy 8.4
J/g, enthalpy 7.7J/g is crystallized, textile process performance is good, and wearability is excellent.
Embodiment 3：
A kind of method that energy-saving and temperature-regulating cellulose fibre is prepared using ionic liquid as solvent, its key step include：
（1）The preparation of the compound porous phase-change material of polyethylene glycol acrylate
Polyethylene glycol acrylate is gathered and melted at 80 DEG C, melts in the backward melt and adds cyclodextrin, medical stone, make
The mass ratio of cyclodextrin, medical stone and polyethylene glycol acrylate three is 5:10:30, blending adsorption time is 2.5h；
（2）The preparation of spinning solution
A, it is blended：It is butyl, the moon by the porous phase-change material of compound polyethylene glycol acrylate of above-mentioned preparation and cation
Ion is SCN-Alkyl imidazole type ionic liquid be blended；
B, it is swelled：By the ionic liquid after blending and the cellulose pulp after crushing by being pre-mixed, wherein obtain
The compound porous phase-change material of polyethylene glycol acrylate in pre-mixed material：Cellulose pulp：The mass ratio of ionic liquid three
For 5:25:70；
C, melt-off：Blending ionic liquid/cellulose pulp compound of preparation is added to twin-screw by charge door and squeezed
Go out machine, the temperature of double screw extruder is 102 DEG C, and screw speed is 122 revs/min, and vacuum is -0.07MPa, in this process
Realize dehydration, deaeration and heating melting；
The spinning solution of above-mentioned preparation is passed through into single screw extrusion machine, the temperature of single screw extrusion machine is 129 DEG C, and screw rod turns
Speed is 101 revs/min, and vacuum is -0.07MPa, spinning solution is further dehydrated, deaeration and mixed melting, Screw Extrusion pressure
Power is 0.65MPa.
（3）Spinning
In the case where Screw Extrusion pressure is 0.65MPa, spinning solution passes through measuring pump, spinneret, is 15% in concentration, temperature
Cation for 37 DEG C is butyl, anion SCN-Alkyl imidazole type ionic liquid coagulating bath in spinning moulding, through drawing-off
Process, wash and the process that oils, the cellulose fibre with phase-changing and temperature-regulating effect is made.
Phase-changing and temperature-regulating cellulose fibre fiber made from embodiment 3 has good phase-changing and temperature-regulating function, melts enthalpy 10.9
J/g, enthalpy 9.2J/g is crystallized, textile process performance is good, and wearability is excellent.
Embodiment 4：
A kind of method that energy-saving and temperature-regulating cellulose fibre is prepared using ionic liquid as solvent, its key step include：
（1）The preparation of the compound porous phase-change material of polyethylene glycol acrylate
Polyethylene glycol acrylate is melted at 90 DEG C, melts in the backward melt and adds molecular sieve, bamboo charcoal, make molecule
Sieve, bamboo charcoal and the mass ratio of polyethylene glycol acrylate three are 20:50:100, blending adsorption time is 3.0h；
（2）The preparation of spinning solution
A, it is blended：Be pi-allyl by the porous phase-change material of compound polyethylene glycol acrylate of above-mentioned preparation and cation,
Anion is SCN-Alkyl imidazole type ionic liquid be blended；
B, it is swelled：By the ionic liquid after blending and the cellulose pulp after crushing by being pre-mixed, wherein obtain
The compound porous phase-change material of polyethylene glycol acrylate in pre-mixed material：Cellulose pulp：The mass ratio of ionic liquid three
For 5:30:65；
C, melt-off：Blending ionic liquid/cellulose pulp compound of preparation is added to twin-screw by charge door and squeezed
Go out machine, the temperature of double screw extruder is 126 DEG C, and screw speed is 96 revs/min, and vacuum is -0.08MPa, real in this process
Dehydration, deaeration and heating melting are showed；
The spinning solution of above-mentioned preparation is passed through into single screw extrusion machine, the temperature of single screw extrusion machine is 138 DEG C, and screw rod turns
Speed is 85 revs/min, and vacuum is -0.07MPa, spinning solution is further dehydrated, deaeration and mixed melting, Screw Extrusion pressure
For 0.82MPa.
（3）Spinning
In the case where Screw Extrusion pressure is 0.82MPa, spinning solution is 9% in concentration, temperature is by measuring pump, spinneret
42 DEG C of cation is pi-allyl, anion SCN-Alkyl imidazole type ionic liquid coagulating bath in spinning moulding, through drawing-off
Process, wash and the process that oils, the cellulose fibre with phase-changing and temperature-regulating effect is made.
Phase-changing and temperature-regulating cellulose fibre fiber made from embodiment 4 has good phase-changing and temperature-regulating function, melts enthalpy 13.4
J/g, enthalpy 11.7J/g is crystallized, textile process performance is good, and wearability is excellent.
Embodiment 5：
A kind of method that energy-saving and temperature-regulating cellulose fibre is prepared using ionic liquid as solvent, its key step include：
（1）The preparation of the compound porous phase-change material of PEO/stearic acid
PEO/stearic acid compound is melted at 100 DEG C, melt added in the backward melt expanded graphite,
Carborundum, the mass ratio for making expanded graphite, carborundum and PEO/stearic acid compound three are 30:50:100, blending
Adsorption time is 4.0h；
（2）The preparation of spinning solution
A, it is blended：It is butyl, the moon by the compound porous phase-change material of PEO/stearic acid of above-mentioned preparation and cation
Ion is CH3COO-Alkyl imidazole type ionic liquid be blended；
B, it is swelled：By the ionic liquid after blending and the cellulose pulp after crushing by being pre-mixed, wherein obtain
The compound porous phase-change material of PEO/stearic acid in pre-mixed material：Cellulose pulp：The mass ratio of ionic liquid three
For 6:30:64；
C, melt-off：Blending ionic liquid/cellulose pulp compound of preparation is added to twin-screw by charge door and squeezed
Go out machine, the temperature of double screw extruder is 149 DEG C, and screw speed is 56 revs/min, and vacuum is -0.10MPa, real in this process
Dehydration, deaeration and heating melting are showed；
The spinning solution of above-mentioned preparation is passed through into single screw extrusion machine, the temperature of single screw extrusion machine is 149 DEG C, and screw rod turns
Speed is 53 revs/min, and vacuum is -0.10MPa, spinning solution is further dehydrated, deaeration and mixed melting, Screw Extrusion pressure
For 0.98MPa.
（3）Spinning
In the case where Screw Extrusion pressure is 0.98MPa, spinning solution is 4% in concentration, temperature is by measuring pump, spinneret
50 DEG C of cation is butyl, anion CH3COO-Alkyl imidazole type ionic liquid coagulating bath in spinning moulding, through drawing-off
Process, wash and the process that oils, the cellulose fibre with phase-changing and temperature-regulating effect is made.
Phase-changing and temperature-regulating cellulose fibre fiber made from embodiment 5 has good phase-changing and temperature-regulating function, melts enthalpy 18.8
J/g, enthalpy 14.5J/g is crystallized, textile process performance is good, and wearability is excellent.
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still may be used
To be modified to the technical scheme described in foregoing embodiments, within the spirit and principles of the invention, that is made appoints
What modification, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (1)
- A kind of 1. phase-changing and temperature-regulating cellulose fibre prepared by solvent method, it is characterised in that：The fiber include porous adsorbing material, Polymeric phase change material and the material with Far-infrared Absorption function；The porous adsorbing material, the material with Far-infrared Absorption function and the mass ratio of polymeric phase change material three are：1 ~30:1~50:10~100；Fibers melt enthalpy >=the 5.5J/g, crystallize enthalpy >=5.3J/g；The porous adsorbing material is a kind of or several in expanded graphite, cyclodextrin, zeolite, molecular sieve, silicate mineral Kind；Described silicate mineral is montmorillonite, diatomite and kaolinic one or more；The material with Far-infrared Absorption function is one kind in graphene, tourmaline, medical stone, bamboo charcoal and carborundum It is or several；The polymeric phase change material is in polyethylene glycol, polyethylene glycol acrylate, PEO/stearic acid compound It is one or more of；Preparation method includes the preparation process of composite high-molecular phase transformation porous material；The preparation process of spinning solution；Spinning process；The preparation process of the composite high-molecular phase transformation porous material, it is by porous adsorbing material, there is Far-infrared Absorption function Material be added to melting complete polymeric phase change material in absorption blending complete；Described polymeric phase change material melting temperature and blending temperature are 60~100 DEG C；The blending adsorption time is 1.0~4.0h；The preparation process of the spinning solution includes blending step, swelling step, melt-off process；The swelling step is that the ionic liquid after blending and the cellulose pulp after crushing are carried out into premixing swelling, is total to Mixed ionic liquid and cellulose pulp compound；In described blending ionic liquid and cellulose pulp compound, composite high-molecular phase transformation porous material：Cellulose pulp： The mass ratio of ionic liquid three is 1~6:15~30:64~84；The melt-off process needs successively to pass through double screw extruder and single screw extrusion machine；In the double screw extruder each section of temperature be 80 ~ 150 DEG C, screw speed be 50 ~ 200 revs/min, vacuum for- 0.05~-0.10MPa；Each section of temperature range is 110 ~ 150 DEG C in the single screw extrusion machine, and screw speed is 50 ~ 120 revs/min, vacuum For -0.05 ~ -0.10MPa, Screw Extrusion pressure is 0.50 ~ 1.0 MPa；In the spinning process, coagulating bath is the distilled water of 30~50 DEG C of temperature, or concentration≤20%, 30~50 DEG C of temperature Ionic liquid used the aqueous solution.
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| CN112440524B (en) * | 2020-11-27 | 2022-08-19 | 江苏科技大学 | Preparation method and application of cellulose double-layer film with phase change-infrared heat dissipation performance |
| CN114874756B (en) * | 2022-07-12 | 2022-09-16 | 北京金羽新能科技有限公司 | Composite phase change material and preparation method and application thereof |
| CN118166440A (en) * | 2024-01-15 | 2024-06-11 | 成都纺织高等专科学校 | Intelligent temperature-regulating silk fiber and preparation method thereof |
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