CN105369380A - 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
- Publication number
- CN105369380A CN105369380A CN201510911769.3A CN201510911769A CN105369380A CN 105369380 A CN105369380 A CN 105369380A CN 201510911769 A CN201510911769 A CN 201510911769A CN 105369380 A CN105369380 A CN 105369380A
- Authority
- CN
- China
- Prior art keywords
- phase
- temperature
- preparation
- changing
- regulating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 53
- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 43
- 239000002904 solvent Substances 0.000 title claims abstract description 25
- 238000009987 spinning Methods 0.000 claims abstract description 50
- 239000012782 phase change material Substances 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 33
- 239000000835 fiber Substances 0.000 claims abstract description 25
- 238000010521 absorption reaction Methods 0.000 claims abstract description 20
- 239000011148 porous material Substances 0.000 claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 10
- 230000008025 crystallization Effects 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000002608 ionic liquid Substances 0.000 claims description 52
- 238000002844 melting Methods 0.000 claims description 31
- 230000008018 melting Effects 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 31
- 229920002678 cellulose Polymers 0.000 claims description 29
- 238000001125 extrusion Methods 0.000 claims description 29
- 239000001913 cellulose Substances 0.000 claims description 28
- 150000001875 compounds Chemical class 0.000 claims description 23
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 22
- -1 poly(ethylene oxide) Polymers 0.000 claims description 22
- 239000002202 Polyethylene glycol Substances 0.000 claims description 18
- 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
- 150000001450 anions Chemical class 0.000 claims description 11
- 150000001768 cations Chemical class 0.000 claims description 11
- 230000009466 transformation Effects 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 7
- 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
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 5
- 229910052604 silicate mineral Inorganic materials 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
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 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
- 239000002808 molecular sieve 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
- 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 4
- 239000004575 stone Substances 0.000 claims description 4
- 229910052613 tourmaline Inorganic materials 0.000 claims description 4
- 229940070527 tourmaline Drugs 0.000 claims description 4
- 239000011032 tourmaline Substances 0.000 claims description 4
- 239000010457 zeolite Substances 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 3
- 229910052736 halogen Inorganic materials 0.000 claims description 3
- 150000002367 halogens Chemical class 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
- CGKQZIULZRXRRJ-UHFFFAOYSA-N Butylone Chemical compound CCC(NC)C(=O)C1=CC=C2OCOC2=C1 CGKQZIULZRXRRJ-UHFFFAOYSA-N 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002689 soil Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 28
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 238000001179 sorption measurement Methods 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract 3
- 230000004927 fusion Effects 0.000 abstract 1
- 230000008961 swelling Effects 0.000 description 10
- 229920000297 Rayon Polymers 0.000 description 8
- 239000004753 textile 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
- 229920000151 polyglycol Polymers 0.000 description 6
- 239000010695 polyglycol Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000000155 melt Substances 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 239000003094 microcapsule Substances 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
- 239000003317 industrial substance Substances 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- 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
- 238000011161 development Methods 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 238000007380 fibre production Methods 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
- 238000011160 research Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004090 dissolution 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
- 230000006872 improvement Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- 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)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (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, relate to a kind of with cellulose pulp and composite phase-change material for raw material, ionic liquid is the phase-changing and temperature-regulating cellulose fibre prepared of solvent and method thereof, belongs to textile technology field.
Technical background
The features such as ionic liquid has that steam forces down, stable performance, non-volatile, favorable solubility, are widely used in the fields such as organic synthesis, electrochemistry, materials chemistry, having good investigation and application prospect.Cellulose receives much concern as eco-friendly renewable resource simultaneously.In recent years, be that one of cellulose fibre emphasis direction becoming this area research prepared by dissolution with solvents cellulose with ionic liquid.
Along with the raising of people's living standard, chemical fibre industry is gradually to functionalization, intelligent direction development, and phase-changing and temperature-regulating fiber is wherein important one.Phase-changing and temperature-regulating fiber utilizes phase-change material discharge in phase transition process or absorb latent heat, thus have two-way automatic temperature-adjusting function.The countries such as America and Europe pay attention to its research and development, and output in domestic is lower, and product, based on import, holds at high price.
Employing microcapsules technology, solution spinning processes are the main method preparing phase-changing and temperature-regulating cellulose fibre, successfully realized at present the phase-changing and temperature-regulating modification of cellulose fibre mainly viscose, as Chinese patent ZL200610157441.8, ZL200710014607.5, ZL200710123411.X, ZL201010164832.9, ZL201010295055.1, ZL201210357126.5,201310420382.9,201410616024.X etc. all discloses the research of viscose temperature adjustment modification.But because microcapsules synthesis technique is complicated in prior art, reaction between solvent and auxiliary agent, cause phase change fiber cost high, functional undesirable, and the flow process of wet spinning technology is longer, inefficiency, simultaneously due in production process of viscose fiber, use NaOH, the industrial chemicals such as carbon disulfide and sulfuric acid, seriously polluted, and in fiber formation process and intervene afterwards process, phase-change material runs off serious, the problems such as energy absorption conversion ratio is not high, so, invent a kind of production procedure pollution-free, product environmental protection and functional good New-type phase change temperature-regulating fiber become urgent problem in our research and development.
Using ionic liquid as cellulosic solvent, activation is not needed during dissolving cellulos, and ionic liquid is easy to reclaim, can be recycled, utilize this system to be convenient to the interpolations such as auxiliary agent simultaneously, and the impact of ionic liquid on auxiliary agent is less, this new varieties being cellulose fibre opens a Tiao Xin road, also solves the problem utilizing viscose process to carry out cellulose CSP to run into very well simultaneously.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, phase-changing and temperature-regulating cellulose fibre providing a kind of solvent method to prepare and preparation method thereof, realizes following goal of the invention:
(1) the phase-changing and temperature-regulating cellulose fibre that obtains of the present invention is to far red light, and visible ray all has absorption, this phase-changing and temperature-regulating fiber is had functional preferably, and the fibers melt enthalpy >=5.5J/g of preparation, crystallization enthalpy >=5.3J/g, textile process performance is good;
(2) utilize porous adsorbing material to adsorb polymeric phase change material, decrease the loss in its forming process, ensure that the phase-changing and temperature-regulating function of fiber, and combine the material with Far-infrared Absorption function, add the absorption to light energy and transformation efficiency;
(3) using ionic liquid as cellulosic solvent, adopt double screw extruder high-temperature digestion to prepare spinning solution, and in conjunction with single screw extrusion machine, improve cellulosic melting effect, achieve cellulose melting, dehydration, vacuum defoamation simultaneously, shorten the time more than 90% relative to viscose process;
(4) preparation method of the present invention, production procedure is short and abandon the synthesis technique of microcapsules complexity, and cost significantly reduces, and production efficiency is high.
(5) compared with viscose process technique, decrease the use of industrial chemicals, realize omnidistance green non-pollution, reduce the environmental hazard of fiber production process, and the harm to operating personnel.
(6) this fiber can extensive use clothes, bedding, medical supplies and nonwoven material field, particularly medical field because raw material, production procedure, product green non-pollution, have wide development space at medical field especially.
The technical scheme that the present invention takes is as follows:
A phase-changing and temperature-regulating cellulose fibre prepared by solvent method, this fiber comprises porous adsorbing material, polymeric phase change material and has the material of Far-infrared Absorption function.
The mass ratio of described porous adsorbing material, the material with Far-infrared Absorption function and polymeric phase change material three is: 1 ~ 30:1 ~ 50:10 ~ 100.
This fibers melt enthalpy >=5.5J/g, crystallization enthalpy >=5.3J/g.
Described porous adsorbing material is one or several in expanded graphite, cyclodextrin, zeolite, molecular sieve, silicate mineral; Described silicate mineral be imvite, diatomite and kaolin soil one or more.
The described material with Far-infrared Absorption function is one or more in Graphene, tourmaline, medical stone, bamboo charcoal and carborundum; Described polymeric phase change material is one or more in polyethylene glycol, polyethylene glycol acrylate, poly(ethylene oxide)/stearic acid compound.
Solvent method prepares a method for phase-changing and temperature-regulating cellulose fibre, comprises the preparation process of composite high-molecular phase transformation porous material; The preparation process of spinning solution; Spinning process.
The preparation of described composite high-molecular phase transformation porous material porous adsorbing material, the material with Far-infrared Absorption function is joined in polymeric phase change material that melting completes to adsorb blended completing.
Described polymeric phase change material melt temperature and blending temperature are 60 ~ 100 ° of C.
Described blended adsorption time is 1.0 ~ 4.0h.
The preparation process of described spinning solution comprises blending step, swelling step, melt-off operation.
In described blending step, the composite high-molecular phase transformation porous material prepared is added alkyl imidazole type ionic liquid, CATION be allyl, ethyl, butyl one or more; Anion is halogen, SCN
-and CH
3cOO
-in one or more, obtain blended after ionic liquid.
Described swelling step be by the ionic liquid after blended with pulverize after cellulose pulp to carry out premixed swelling, obtain blended ionic liquid and cellulose pulp compound.
Composite high-molecular phase transformation porous material in described blended ionic liquid and cellulose pulp compound: cellulose pulp: the mass ratio of ionic liquid three is 1 ~ 6:15 ~ 30:64 ~ 84.
Described melt-off operation needs successively through double screw extruder and single screw extrusion machine.
In described double screw extruder, the temperature of each section is 80 ~ 150 DEG C, screw speed is 50 ~ 200 revs/min, vacuum is-0.05 ~-0.10Mpa, in described single screw extrusion machine, the temperature range of each section is 110 ~ 150 DEG C, screw speed is 50 ~ 120 revs/min, vacuum is-0.05 ~-0.10MPa, and Screw Extrusion pressure is 0.50 ~ 1.0MPa.
In described spinning process, coagulating bath is the distilled water of temperature 30 ~ 50 DEG C, or is concentration≤20%, the aqueous solution of the ionic liquid used of temperature 30 ~ 50 DEG C.
The mass ratio of described porous adsorbing material, the material with Far-infrared Absorption function and polymeric phase change material three is: 1 ~ 30:1 ~ 50:10 ~ 100.
In process of production, can according to the needs produced and requirement to product, suitable adjustment is carried out to the preparation technology of spinning solution, spinning technique and aftertreatment technology.
The invention provides a kind of method taking ionic liquid as the spinning technique of solvent and prepare phase-changing and temperature-regulating cellulose fibre, phase-changing and temperature-regulating cellulose fibre prepared by the method is on the basis based on polymeric phase change material, porous material is utilized to be adsorbed by polymeric phase change material melt, and combine the material with Far-infrared Absorption function, prepare composite high-molecular phase transformation porous material, by the composite high-molecular phase transformation porous material of above-mentioned preparation and ionic liquid blended, and cellulose pulp is mixed with above-mentioned blended liquid, adopting screw extrusion method to obtain take ionic liquid as the spinning solution of solvent, solvent spinning technique is utilized to prepare the energy-saving and temperature-regulating cellulose fibre of high enthalpy, there is production procedure pollution-free, the feature of product environmental protection.
The present invention adopts the beneficial effect of technique scheme:
(1) the phase-changing and temperature-regulating cellulose fibre that obtains of the present invention is to far red light, and visible ray all has absorption, the fibers melt enthalpy >=5.5J/g of preparation, crystallization enthalpy >=5.3J/g, and textile process performance is good;
(2) utilize porous adsorbing material to adsorb polymeric phase change material, decrease the loss in its forming process, ensure that the phase-changing and temperature-regulating function of fiber, and combine the material with Far-infrared Absorption function, add the absorption to light energy and transformation efficiency;
(3) using ionic liquid as cellulosic solvent, adopt double screw extruder high-temperature digestion to prepare spinning solution, and in conjunction with single screw extrusion machine, improve cellulosic melting effect, achieve cellulose melting, dehydration, vacuum defoamation, the shortening time 90% compared with viscose process simultaneously;
(4) preparation method of the present invention, production procedure is short and abandon the synthesis technique of microcapsules complexity, and cost significantly reduces, and technological process is short, production efficiency is high.
(5) compared with viscose process technique, decrease the use of industrial chemicals, realize omnidistance green non-pollution, reduce the environmental hazard of fiber production process, and the harm to operating personnel.
Below in conjunction with embodiment, the present invention is described in detail.
Detailed description of the invention
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
Content percentage in embodiment is mass percent.
embodiment 1:
Take ionic liquid as the method that energy-saving and temperature-regulating cellulose fibre prepared by solvent, its key step comprises:
(1) preparation of the polyglycol porous phase-change material of compound
By polyethylene glycol melting at 60 DEG C, add silicate mineral-imvite, tourmaline in melting this melt backward, make silicate mineral, the mass ratio of tourmaline and polyethylene glycol three is 1:1:10, blended adsorption time is 1.0h;
(2) preparation of spinning solution
A, blended: to be allyl by polyglycol porous for the compound of above-mentioned preparation phase-change material and CATION, anion is that the alkyl imidazole type ionic liquid of halogen carries out blended;
B, swelling: by the ionic liquid after blended with pulverize after cellulose pulp to carry out premixed in proportion swelling, the polyglycol porous phase-change material of compound in the premixed material wherein obtained: cellulose pulp: the mass ratio of ionic liquid three is 1:15:84;
C, melt-off: the blended ionic liquid/cellulose pulp compound of preparation is joined double screw extruder by charge door, the temperature of double screw extruder is 80 DEG C, screw speed is 200 revs/min, vacuum is-0.05MPa, dehydration, deaeration and heating and melting at this process implementation;
By the spinning solution of above-mentioned preparation through single screw extrusion machine, the temperature of single screw extrusion machine is 110 DEG C, and screw speed is 120 revs/min, and vacuum is-0.05MPa, spinning solution is dewatered further, deaeration and mixed melting, Single screw extrusion pressure is 0.50MPa.
(3) spinning
Under Single screw extrusion pressure is 0.50MPa, by spinning solution through measuring pump, spinnerets, be spinning moulding in 35 DEG C of distilled water coagulating baths in temperature, through drafting process, operation of washing and oil, the obtained cellulose fibre with phase-changing and temperature-regulating effect.
The phase-changing and temperature-regulating cellulose fibre fiber that embodiment 1 obtains has good phase-changing and temperature-regulating function, melting enthalpy 5.5J/g, and crystallization enthalpy 5.3J/g, textile process performance is good, and wearability is excellent.
embodiment 2:
Take ionic liquid as the method that energy-saving and temperature-regulating cellulose fibre prepared by solvent, its key step comprises:
(1) preparation of the polyglycol porous phase-change material of compound
By polyethylene glycol melting at 70 DEG C, add zeolite, Graphene in melting this melt backward, make zeolite, the mass ratio of Graphene and polyethylene glycol three is 1:2:20, blended adsorption time is 2.0h;
(2) preparation of spinning solution
A, blended: to be ethyl by polyglycol porous for the compound of above-mentioned preparation phase-change material and CATION, anion is CH
3cOO
-alkyl imidazole type ionic liquid carry out blended;
B, swelling: by the ionic liquid after blended with pulverize after cellulose pulp swelling by carrying out premixed, the polyglycol porous phase-change material of compound in the premixed material wherein obtained: cellulose pulp: the mass ratio of ionic liquid three is 2:20:78;
C, melt-off: the blended ionic liquid/cellulose pulp compound of preparation is joined double screw extruder by charge door, the temperature of double screw extruder is 89 DEG C, screw speed is 176 revs/min, vacuum is-0.06MPa, dehydration, deaeration and heating and melting at this process implementation;
By the spinning solution of above-mentioned preparation through single screw extrusion machine, the temperature of single screw extrusion machine is 118 DEG C, and screw speed is 112 revs/min, and vacuum is-0.06MPa, spinning solution is dewatered further, deaeration and mixed melting, and Screw Extrusion pressure is 0.57MPa.
(3) spinning
Under Screw Extrusion pressure is 0.57MPa, spinning solution, through measuring pump, spinnerets, is 20% in concentration, and temperature is that the CATION of 31 DEG C is ethyl, anion is CH
3cOO
-alkyl imidazole type ionic liquid coagulating bath in spinning moulding, through drafting process, operation of washing and oil, the obtained cellulose fibre with phase-changing and temperature-regulating effect.
The phase-changing and temperature-regulating cellulose fibre fiber that embodiment 2 obtains has good phase-changing and temperature-regulating function, melting enthalpy 8.4J/g, and crystallization enthalpy 7.7J/g, textile process performance is good, and wearability is excellent.
embodiment 3:
Take ionic liquid as the method that energy-saving and temperature-regulating cellulose fibre prepared by solvent, its key step comprises:
(1) preparation of compound polyethylene glycol acrylate porous phase-change material
Polyethylene glycol acrylate is gathered melting at 80 DEG C, adds cyclodextrin, medical stone in melting this melt backward, make cyclodextrin, the mass ratio of medical stone and polyethylene glycol acrylate three is 5:10:30, blended adsorption time is 2.5h;
(2) preparation of spinning solution
A, blended: to be butyl by the compound polyethylene glycol acrylate porous phase-change material of above-mentioned preparation and CATION, anion is SCN
-alkyl imidazole type ionic liquid carry out blended;
B, swelling: by the ionic liquid after blended with pulverize after cellulose pulp by carrying out premixed, compound polyethylene glycol acrylate porous phase-change material in the premixed material wherein obtained: cellulose pulp: the mass ratio of ionic liquid three is 5:25:70;
C, melt-off: the blended ionic liquid/cellulose pulp compound of preparation is joined double screw extruder by charge door, the temperature of double screw extruder is 102 DEG C, screw speed is 122 revs/min, vacuum is-0.07MPa, dehydration, deaeration and heating and melting at this process implementation;
By the spinning solution of above-mentioned preparation through single screw extrusion machine, the temperature of single screw extrusion machine is 129 DEG C, and screw speed is 101 revs/min, and vacuum is-0.07MPa, spinning solution is dewatered further, deaeration and mixed melting, and Screw Extrusion pressure is 0.65MPa.
(3) spinning
Under Screw Extrusion pressure is 0.65MPa, spinning solution, through measuring pump, spinnerets, is 15% in concentration, and temperature is that the CATION of 37 DEG C is butyl, anion is SCN
-alkyl imidazole type ionic liquid coagulating bath in spinning moulding, through drafting process, operation of washing and oil, the obtained cellulose fibre with phase-changing and temperature-regulating effect.
The phase-changing and temperature-regulating cellulose fibre fiber that embodiment 3 obtains has good phase-changing and temperature-regulating function, melting enthalpy 10.9J/g, and crystallization enthalpy 9.2J/g, textile process performance is good, and wearability is excellent.
embodiment 4:
Take ionic liquid as the method that energy-saving and temperature-regulating cellulose fibre prepared by solvent, its key step comprises:
(1) preparation of compound polyethylene glycol acrylate porous phase-change material
By polyethylene glycol acrylate melting at 90 DEG C, add molecular sieve, bamboo charcoal in melting this melt backward, make molecular sieve, the mass ratio of bamboo charcoal and polyethylene glycol acrylate three is 20:50:100, blended adsorption time is 3.0h;
(2) preparation of spinning solution
A, blended: to be allyl by the compound polyethylene glycol acrylate porous phase-change material of above-mentioned preparation and CATION, anion is SCN
-alkyl imidazole type ionic liquid carry out blended;
B, swelling: by the ionic liquid after blended with pulverize after cellulose pulp by carrying out premixed, compound polyethylene glycol acrylate porous phase-change material in the premixed material wherein obtained: cellulose pulp: the mass ratio of ionic liquid three is 5:30:65;
C, melt-off: the blended ionic liquid/cellulose pulp compound of preparation is joined double screw extruder by charge door, the temperature of double screw extruder is 126 DEG C, screw speed is 96 revs/min, vacuum is-0.08MPa, dehydration, deaeration and heating and melting at this process implementation;
By the spinning solution of above-mentioned preparation through single screw extrusion machine, the temperature of single screw extrusion machine is 138 DEG C, and screw speed is 85 revs/min, and vacuum is-0.07MPa, spinning solution is dewatered further, deaeration and mixed melting, and Screw Extrusion pressure is 0.82MPa.
(3) spinning
Under Screw Extrusion pressure is 0.82MPa, spinning solution, through measuring pump, spinnerets, is 9% in concentration, and temperature is that the CATION of 42 DEG C is allyl, anion is SCN
-alkyl imidazole type ionic liquid coagulating bath in spinning moulding, through drafting process, operation of washing and oil, the obtained cellulose fibre with phase-changing and temperature-regulating effect.
The phase-changing and temperature-regulating cellulose fibre fiber that embodiment 4 obtains has good phase-changing and temperature-regulating function, melting enthalpy 13.4J/g, and crystallization enthalpy 11.7J/g, textile process performance is good, and wearability is excellent.
embodiment 5:
Take ionic liquid as the method that energy-saving and temperature-regulating cellulose fibre prepared by solvent, its key step comprises:
(1) preparation of compound poly(ethylene oxide)/stearic acid porous phase-change material
By poly(ethylene oxide)/stearic acid compound melting at 100 DEG C, expanded graphite, carborundum is added in melting this melt backward, make the mass ratio of expanded graphite, carborundum and poly(ethylene oxide)/stearic acid compound three be 30:50:100, blended adsorption time is 4.0h;
(2) preparation of spinning solution
A, blended: to be butyl by the compound of above-mentioned preparation poly(ethylene oxide)/stearic acid porous phase-change material and CATION, anion is CH
3cOO
-alkyl imidazole type ionic liquid carry out blended;
B, swelling: by the ionic liquid after blended with pulverize after cellulose pulp by carrying out premixed, compound poly(ethylene oxide)/stearic acid porous phase-change material in the premixed material wherein obtained: cellulose pulp: the mass ratio of ionic liquid three is 6:30:64;
C, melt-off: the blended ionic liquid/cellulose pulp compound of preparation is joined double screw extruder by charge door, the temperature of double screw extruder is 149 DEG C, screw speed is 56 revs/min, vacuum is-0.10MPa, dehydration, deaeration and heating and melting at this process implementation;
By the spinning solution of above-mentioned preparation through single screw extrusion machine, the temperature of single screw extrusion machine is 149 DEG C, and screw speed is 53 revs/min, and vacuum is-0.10MPa, spinning solution is dewatered further, deaeration and mixed melting, and Screw Extrusion pressure is 0.98MPa.
(3) spinning
Under Screw Extrusion pressure is 0.98MPa, spinning solution, through measuring pump, spinnerets, is 4% in concentration, and temperature is that the CATION of 50 DEG C is butyl, anion is CH
3cOO
-alkyl imidazole type ionic liquid coagulating bath in spinning moulding, through drafting process, operation of washing and oil, the obtained cellulose fibre with phase-changing and temperature-regulating effect.
The phase-changing and temperature-regulating cellulose fibre fiber that embodiment 5 obtains has good phase-changing and temperature-regulating function, melting enthalpy 18.8J/g, and crystallization enthalpy 14.5J/g, textile process performance is good, and wearability is excellent.
Last it is noted that the foregoing is only the preferred embodiments of the present invention; be not limited to the present invention; although with reference to previous embodiment to invention has been detailed description; for a person skilled in the art; it still can be modified to the technical scheme described in foregoing embodiments; within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the phase-changing and temperature-regulating cellulose fibre prepared of solvent method, is characterized in that: this fiber comprises porous adsorbing material, polymeric phase change material and has the material of Far-infrared Absorption function.
2. the phase-changing and temperature-regulating cellulose fibre prepared of a kind of solvent method according to claim 1, is characterized in that: the mass ratio of described porous adsorbing material, the material with Far-infrared Absorption function and polymeric phase change material three is: 1 ~ 30:1 ~ 50:10 ~ 100.
3. the phase-changing and temperature-regulating cellulose fibre prepared of a kind of solvent method according to claim 1, is characterized in that: this fibers melt enthalpy >=5.5J/g, crystallization enthalpy >=5.3J/g.
4. the phase-changing and temperature-regulating cellulose fibre prepared of a kind of solvent method according to claim 1, is characterized in that: described porous adsorbing material is one or several in expanded graphite, cyclodextrin, zeolite, molecular sieve, silicate mineral; Described silicate mineral be imvite, diatomite and kaolin soil one or more;
The described material with Far-infrared Absorption function is one or more in Graphene, tourmaline, medical stone, bamboo charcoal and carborundum;
Described polymeric phase change material is one or more in polyethylene glycol, polyethylene glycol acrylate, poly(ethylene oxide)/stearic acid compound.
5. solvent method prepares a method for phase-changing and temperature-regulating cellulose fibre, it is characterized in that: the preparation process comprising composite high-molecular phase transformation porous material; The preparation process of spinning solution; Spinning process.
6. the preparation method of phase-changing and temperature-regulating cellulose fibre according to claim 5, is characterized in that: the preparation process of described spinning solution comprises melt-off operation, and described melt-off operation needs successively through double screw extruder and single screw extrusion machine.
7. the preparation method of phase-changing and temperature-regulating cellulose fibre according to claim 5, is characterized in that: in described double screw extruder, the temperature of each section is 80 ~ 150 DEG C, and screw speed is 50 ~ 200 revs/min, and vacuum is-0.05 ~-0.10Mpa.
8. the preparation method of phase-changing and temperature-regulating cellulose fibre according to claim 5, it is characterized in that: in described single screw extrusion machine, the temperature range of each section is 110 ~ 150 DEG C, screw speed is 50 ~ 120 revs/min, and vacuum is-0.05 ~-0.10MPa, and Screw Extrusion pressure is 0.50 ~ 1.0MPa.
9. the preparation method of phase-changing and temperature-regulating cellulose fibre according to claim 5, is characterized in that: the preparation process of described composite high-molecular phase transformation porous material porous adsorbing material, the material with Far-infrared Absorption function is joined in polymeric phase change material that melting completes to adsorb blended completing.
10. the preparation method of phase-changing and temperature-regulating cellulose fibre according to claim 4, is characterized in that:
The preparation process of described spinning solution comprises blending step, and in described blending step, the ionic liquid added is alkyl imidazole type ionic liquid, CATION be allyl, ethyl, butyl one or more; Anion is halogen, SCN
-and CH
3cOO
-in one or more;
In described spinning process, coagulating bath is the distilled water of temperature 30 ~ 50 DEG C, or concentration≤20%, temperature 30 ~ 50 DEG C the aqueous solution of ionic liquid used;
In the preparation process of described spinning solution, composite high-molecular phase transformation porous material in blended ionic liquid and cellulose pulp compound: cellulose pulp: the mass ratio of ionic liquid three is 1 ~ 6:15 ~ 30:64 ~ 84.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510911769.3A CN105369380B (en) | 2015-12-11 | 2015-12-11 | Phase-change temperature-regulating cellulose fiber prepared by solvent method and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510911769.3A CN105369380B (en) | 2015-12-11 | 2015-12-11 | Phase-change temperature-regulating cellulose fiber prepared by solvent method and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105369380A true CN105369380A (en) | 2016-03-02 |
| CN105369380B CN105369380B (en) | 2017-12-22 |
Family
ID=55371994
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510911769.3A Active CN105369380B (en) | 2015-12-11 | 2015-12-11 | Phase-change temperature-regulating cellulose fiber prepared by solvent method and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105369380B (en) |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106467985A (en) * | 2016-03-04 | 2017-03-01 | 济南圣泉集团股份有限公司 | Refreshing regenerated celulose fibre of a kind of ice and preparation method thereof and textile |
| CN106637455A (en) * | 2017-01-19 | 2017-05-10 | 何竞钟 | Processing process and weaving process of functional fibers |
| CN107460596A (en) * | 2017-08-04 | 2017-12-12 | 宁波黄古林工艺品有限公司 | A kind of bamboo fibre summer sleeping mat and preparation method thereof |
| CN107675286A (en) * | 2017-09-28 | 2018-02-09 | 武汉纺织大学 | Orange petal type temperature-adjusting energy-storage phase change fiber and preparation method thereof |
| CN108677265A (en) * | 2018-05-17 | 2018-10-19 | 四川大学 | A kind of filament shape fibrous material and preparation method thereof containing macrocyclic compounds |
| CN108822343A (en) * | 2018-04-25 | 2018-11-16 | 武汉水木弘新材料有限公司 | A kind of preparation method of phase transformation material of regenerated cellulose |
| CN109576808A (en) * | 2018-11-29 | 2019-04-05 | 山传雷 | A kind of inorganic fire-retarded intelligent temperature adjusting fiber cellulose fiber and preparation method thereof |
| CN109825896A (en) * | 2019-02-27 | 2019-05-31 | 温州优巴信息技术有限公司 | A kind of phase-change accumulation energy regenerated celulose fibre and preparation method thereof that hollow porous gelatin methacryl is modified |
| CN112086704A (en) * | 2019-06-12 | 2020-12-15 | 中国石油化工股份有限公司 | Power battery heat dissipation device based on ionic liquid phase-change material |
| CN112440524A (en) * | 2020-11-27 | 2021-03-05 | 江苏科技大学 | Preparation method and application of cellulose double-layer film with phase change-infrared heat dissipation performance |
| CN109505027B (en) * | 2018-11-29 | 2021-11-30 | 上海绿薇生物科技有限公司 | High-sensitivity heat-conducting air conditioner fiber and preparation method thereof |
| CN113897016A (en) * | 2020-06-22 | 2022-01-07 | 佛山品特塑彩新材料有限公司 | Super-weather-resistant functional film and preparation method thereof |
| CN114874756A (en) * | 2022-07-12 | 2022-08-09 | 北京金羽新能科技有限公司 | Composite phase-change material and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101451307A (en) * | 2007-12-06 | 2009-06-10 | 华楙生化科技股份有限公司 | Long acting cooling composite powder, cooling fiber and method for producing the same |
| CN101595258A (en) * | 2007-01-10 | 2009-12-02 | 皮卡地毛纺公司 | Textile substrate is by the functionizing method of bridging under ionisation radiation |
| CN102561027A (en) * | 2011-12-23 | 2012-07-11 | 宏大研究院有限公司 | Wadding flake with function of intellectualized thermoregulation and preparation method thereof |
| CN103060938A (en) * | 2012-11-26 | 2013-04-24 | 浙江理工大学 | Method for manufacturing functional viscose fibers |
| CN103243406A (en) * | 2013-05-22 | 2013-08-14 | 东华大学 | Method for preparing intelligent temperature regulation fiber by melt spinning process |
| CN104178843A (en) * | 2014-07-30 | 2014-12-03 | 滁州惠智科技服务有限公司 | Phase change blend fiber and production method thereof |
-
2015
- 2015-12-11 CN CN201510911769.3A patent/CN105369380B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101595258A (en) * | 2007-01-10 | 2009-12-02 | 皮卡地毛纺公司 | Textile substrate is by the functionizing method of bridging under ionisation radiation |
| CN101451307A (en) * | 2007-12-06 | 2009-06-10 | 华楙生化科技股份有限公司 | Long acting cooling composite powder, cooling fiber and method for producing the same |
| CN102561027A (en) * | 2011-12-23 | 2012-07-11 | 宏大研究院有限公司 | Wadding flake with function of intellectualized thermoregulation and preparation method thereof |
| CN103060938A (en) * | 2012-11-26 | 2013-04-24 | 浙江理工大学 | Method for manufacturing functional viscose fibers |
| CN103243406A (en) * | 2013-05-22 | 2013-08-14 | 东华大学 | Method for preparing intelligent temperature regulation fiber by melt spinning process |
| CN104178843A (en) * | 2014-07-30 | 2014-12-03 | 滁州惠智科技服务有限公司 | Phase change blend fiber and production method thereof |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106467985B (en) * | 2016-03-04 | 2019-08-06 | 济南圣泉集团股份有限公司 | A kind of ice is felt well regenerated celulose fibre and preparation method thereof and textile |
| CN106467985A (en) * | 2016-03-04 | 2017-03-01 | 济南圣泉集团股份有限公司 | Refreshing regenerated celulose fibre of a kind of ice and preparation method thereof and textile |
| CN106637455A (en) * | 2017-01-19 | 2017-05-10 | 何竞钟 | Processing process and weaving process of functional fibers |
| CN107460596A (en) * | 2017-08-04 | 2017-12-12 | 宁波黄古林工艺品有限公司 | A kind of bamboo fibre summer sleeping mat and preparation method thereof |
| CN107675286A (en) * | 2017-09-28 | 2018-02-09 | 武汉纺织大学 | Orange petal type temperature-adjusting energy-storage phase change fiber and preparation method thereof |
| CN107675286B (en) * | 2017-09-28 | 2020-04-14 | 武汉纺织大学 | Orange segment type temperature-regulating energy-storage phase-change fiber and preparation method thereof |
| CN108822343A (en) * | 2018-04-25 | 2018-11-16 | 武汉水木弘新材料有限公司 | A kind of preparation method of phase transformation material of regenerated cellulose |
| CN108677265A (en) * | 2018-05-17 | 2018-10-19 | 四川大学 | A kind of filament shape fibrous material and preparation method thereof containing macrocyclic compounds |
| CN109576808A (en) * | 2018-11-29 | 2019-04-05 | 山传雷 | A kind of inorganic fire-retarded intelligent temperature adjusting fiber cellulose fiber and preparation method thereof |
| CN109576808B (en) * | 2018-11-29 | 2021-08-24 | 青岛邦特生态纺织科技有限公司 | Inorganic flame-retardant intelligent temperature-adjusting cellulose fiber and preparation method thereof |
| CN109505027B (en) * | 2018-11-29 | 2021-11-30 | 上海绿薇生物科技有限公司 | High-sensitivity heat-conducting air conditioner fiber and preparation method thereof |
| CN109825896A (en) * | 2019-02-27 | 2019-05-31 | 温州优巴信息技术有限公司 | A kind of phase-change accumulation energy regenerated celulose fibre and preparation method thereof that hollow porous gelatin methacryl is modified |
| CN112086704A (en) * | 2019-06-12 | 2020-12-15 | 中国石油化工股份有限公司 | Power battery heat dissipation device based on ionic liquid phase-change material |
| CN113897016A (en) * | 2020-06-22 | 2022-01-07 | 佛山品特塑彩新材料有限公司 | Super-weather-resistant functional film and preparation method thereof |
| CN112440524A (en) * | 2020-11-27 | 2021-03-05 | 江苏科技大学 | Preparation method and application of cellulose double-layer film with phase change-infrared heat dissipation performance |
| 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 |
| CN114874756A (en) * | 2022-07-12 | 2022-08-09 | 北京金羽新能科技有限公司 | Composite phase-change material and preparation method and application thereof |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105369380B (en) | 2017-12-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105369380A (en) | Phase-change temperature-regulating cellulose fiber prepared by solvent method and preparation method thereof | |
| CN106149083B (en) | Functional graphene cellulose fiber prepared by melting method and preparation method thereof | |
| CN101838861B (en) | Method for preparing cellulose fiber | |
| CN101492837B (en) | Process for producing bacteria cellulose fibre with high degree of polymerization | |
| CN100339519C (en) | Method of preparing high performance polyvinyl alcohel fiber | |
| CN103173892B (en) | A kind of preparation method of nano bamboo fiber composite material | |
| CN101220522B (en) | Method for manufacturing cellulose/ion liquid spinning liquid with double-screw extrusion machine | |
| CN102154720A (en) | Preparation method of cellulose fibres | |
| CN103031611B (en) | A kind of vinal and its preparation method and application | |
| CN103409837B (en) | The method of water-soluble polyvinyl alcohol fibers prepared by a kind of melt spinning | |
| CN103469588B (en) | The preparation method of the agent of sisal fiber surface size and sisal fiber composite | |
| CN103305952B (en) | Preparation of cellulose spinning solution | |
| CN101230493A (en) | Solvent preparation cellulose bamboo charcoal fibre and use thereof | |
| CN101994168A (en) | Method for preparing high-strength carrageenin fibers | |
| CN101942705A (en) | Preparation method of regenerated bacterial cellulose fiber | |
| CN101580969A (en) | Heat-storage warm-keeping cellulose fiber and preparation method thereof | |
| CN102965752B (en) | Cellulose in-situ urea modified plastification melt spinning method | |
| CN106398129A (en) | Self-adjusting and hygroscopic modified polyester synthesis method | |
| CN102220660B (en) | Method for preparing high phase transition enthalpy phase transition temperature-adjusting fiber from hydrolysis products of waste acrylic yarn | |
| CN104194059A (en) | Cellulose thermoplastic material and preparation method thereof | |
| CN102677218B (en) | Anti-ultraviolet polyphenyl thioether filament and preparation method thereof | |
| CN109440223A (en) | A kind of wet fiber material preparation method of spiral porous structure | |
| CN103290508B (en) | Waste cotton textile regeneration spinning solution formulation and wet spinning process | |
| CN115772713A (en) | Method for preparing PVA (polyvinyl alcohol) coarse denier fiber through melt plasticization-wet spinning | |
| CN105002582B (en) | A kind of preparation method of Chinese mugwort cellulose spin dope |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20220519 Address after: 261106 north of Xinsha Road, Guti street, Hanting District, Weifang City, Shandong Province Patentee after: Weifang Xinlong biomaterials Co.,Ltd. Address before: 261100 building 89, 1825 Hailong Road, Hanting District, Weifang City, Shandong Province Patentee before: HENGTIAN HAILONG (WEIFANG) NEW MATERIALS CO.,LTD. |