CN101748511A - Preparation method of temperature response macromolecular gelatinous fibre material and products thereof - Google Patents
Preparation method of temperature response macromolecular gelatinous fibre material and products thereof Download PDFInfo
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- CN101748511A CN101748511A CN200910229169A CN200910229169A CN101748511A CN 101748511 A CN101748511 A CN 101748511A CN 200910229169 A CN200910229169 A CN 200910229169A CN 200910229169 A CN200910229169 A CN 200910229169A CN 101748511 A CN101748511 A CN 101748511A
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Abstract
The invention relates to a preparation method of temperature response macromolecular gelatinous fibre material and products thereof, which can be applied on artificial muscles. Temperature response gelatinous fibre is produced by the mutual penetrating mixture of poly (N-isopropylacrylamide) and polyvinyl alcohol by a wet spinning process. The poly (N-isopropylacrylamide) and the polyvinyl alcohol are respectively 5 percent to 25percent by weight percent. The preparation method comprises the following three steps: 1, utilizing an in-situ polymerization method to polymerize the poly (N-isopropylacrylamide) in a polyvinyl alcohol water solution system, and preparing polyvinyl alcohol/ poly (N-isopropylacrylamide) spinning solution; 2, taking saturation ammonium persulfate solution as coagulating bath, and utilizing the wet spinning process to prepare polyvinyl alcohol/ poly (N-isopropylacrylamide) primary gelatinous fibre; and 3, carrying out vacuum heat treatment on the primary gelatinous fibre, and improving the heat resistance and structural stability of the primary gelatinous fibre. Compared with the traditional temperature response gelatinous fibre, the polyvinyl alcohol/ poly (N-isopropylacrylamide) primary gelatinous fibre of the invention has good strength, rapid response speed, good biocompatibility, and wide application prospect on the artificial muscles and other biological fields.
Description
Technical field
The present invention relates to the intelligent polymer material technology, be specially temperature-sensitive macromolecular gel fiber material that a kind of IPN blend by poly-N-isopropyl acrylamide (PNIPAAm) and polyvinyl alcohol (PVA) that can be used for artificial-muscle makes by wet spinning technology and preparation method thereof technology.Belong to filed of functional.
Background technology
Artificial-muscle is meant without mechanical device, and the material that drives with electric field driven or chemistry.The material that is used to prepare artificial-muscle at present has high-molecular gel, conducting polymer composite, liquid crystal high polymer material, supermolecule system, metal-polymer composite etc.Wherein, high-molecular gel has caused concern widely with excellent biological compatibility.High-molecular gel is the multicomponent system by polymer three-dimensional network and solvent composition, to environmental stimulus such as temperature, pH, electric field, solvent property, luminous intensity and optical wavelength, pressure, ionic strength, ion concentration and special chemical stimulation (as sugar) etc., produce the polymer network of great variety in shape in macroscopic view (volume).The response process of gel can directly change into mechanical energy with chemical energy, and the process of this power conversion is often seen in organism.Scientists is thought: except that animal muscle, having macromolecule hydrogel only is to can be used for the ideal material of chemical energy to the mechanical energy conversion.
Gel is used in the artificial-muscle aspect early research, and in the ascendant so far.As far back as eighties of last century eighties, Suzuki (the M.Suzuki of Japan, Kobunshi Ronbunshu.46 (1989), 603.) weakly acidic polyacrylic acid (PAA) and weakly alkaline polyarylamine (PAIAM) hydrochloride are mixed, thawing after freezing makes it gelation, last has promptly obtained the rapid-action material with acid, the alkali cleaning of 0.001g/ml repeatedly.This material is placed on as the artificial-muscle wrist carries out elongation test in the water, when adding acetone, " wrist " lifts, and carries heavy 40g immediately, and be closely similar with the action of people's wrist.
Gong (Y.H.Na, Y.Katsuyama, J.P.Gong.Surf Sci Nanotech.3 (2005), 8.) etc. the method for human chemical crosslinking has prepared poly-(2-acrylamido-2-methyl propane sulfonic acid/acrylamide) and (PAMPS/PDMAAm) has waited double-layer network aquogel, this gel fracture strength reaches 10-40MPa, be hundreds of times of component gel, Gong etc. is being that target advances gel in the application aspect the artificial-muscle with joint prosthesis and artificial cartilage just at present.
Though Many researchers is all explored in the application aspect biological tissue and the artificial muscle gel, all be conception and simple modelling mostly, the example of practical application is still rare.Data shows: the time to irritant reaction when skeletal muscle fiber single shaft shrinks is 30ms, then is 100-200ms if load shrinks, and the tension force of generation is 5-10kg/cm
2, shrinkage factor reaches 50%.More than these numerical value are desired values that the mechanical property of material performance muscle should reach.Compare with animal muscle, the response speed of gel and mechanical property also do not reach requirement.Such as: gel rubber material commonly used needed about 50s the time of irritant reaction, with reaction time of skeletal muscle big gap was arranged.In addition, the moisture that gel is high makes and is easy to fragmentation in its use, and as the artificial thews material that load is usually shunk the favorable mechanical performance must be arranged, and this also is a major reason of restriction gel application.
In view of the defective of gel in application aspect the artificial-muscle, the someone attempts having prepared fibrous gel, and just gelatinous fibre (hydrogel fiber) is to improve the application performance of gel.Schreyer (M.Shahinpoor, K.J.Kim, M.Mojarrad, Taylor ﹠amp as U.S. University of New Mexico; Francis Press.NewYork, ch.1 (2007) .) etc. human PAN platinum plating gelatinous fibre do electrode, extruding force surpasses natural muscle.Alternately add bronsted lowry acids and bases bronsted lowry, reversible contraction and swelling take place in this fiber, and chemical energy is converted into mechanical energy.Length variations is about 80%, and the systole response time is less than 2s.At present, U.S. University of New Mexico is using the direct heart-assist device of this developing material electronics muscle formula.
Domestic hair Lijing (L.J.Mao, Y.J.Hu, Y.S.Piao, X.D.Chen, W.S.Xian andD.X.Piao, Curr Appl Phys.5 (2005), 426.) etc. the method by surface grafting PAN is grafted on the fiber of shitosan, the PAN to grafting is hydrolyzed then, has prepared artificial-muscle, this artificial-muscle just can shrink in 20s-30s in methanol solution, just can expand less than 10s in water.Hair etc. has also been made fiber fabric and has been studied its response performance.
[L.w.Yu, J.Y.Xu, L.X.Gu, Polym Int57 (2008), 1017.] such as the Gu Lixia of Donghua University are doing a lot of useful explorations aspect the preparation of gelatinous fibre and the performance study.This seminar carries out alkaline hydrolysis with polyacrylonitrile (PAN) in the NaOH aqueous solution, then with blend such as soybean protein isolate (SPI) and gelatin, be extruded in the coagulating bath solidify, crosslinked, preparation hydrolyzed polyacrylonitrile (HPAN)/SPI and (HPAN)/Ge aquagel fibre.By measuring the equilibrium swelling percentage elongation of gelatinous fibre under different pH, observe gelatinous fibre and lag behind and reversible stretch/shrink behavior.
Compare with conventional gel, the application of gelatinous fibre aspect artificial-muscle has following advantage:
1, more similar to the structure of animal muscle.The musculature of animal mainly is made up of myocyte's (muscle fibre), and other compositions also have blood vessel, nerve and a spot of connective tissue.If fritter skeletal muscle sliced meat are analyzed to molecular level (temporarily ignoring non-muscle fibre component), see that then it is the multilayered structure system that is arranged in parallel and is formed by the fiber (bundle) that thickness does not wait, the member of all levels all is fibrous (elongated cylinder), gel is made fibrous, structurally more similar to animal muscle, help the application of gel in artificial-muscle.
2, mechanical property can strengthen greatly.Fibrous material possesses mechanical performance preferably owing to structurally have higher orientation and crystallization, and gel rubber material and fibrous material are combined, and will improve the mechanical property of material greatly.
3, response speed can increase.Square being directly proportional of required time of gel contraction or expansion and sample size becomes small-sized fiber with traditional block preparing gel, will improve the speed of response of material greatly.
At present, focus mostly at electroresponse and pH responsive materials for gelatinous fibre, and fewer to the gelatinous fibre research of temperature-responsive.The applicant once utilized the method for in-situ polymerization to prepare the PNIPAAm/PVA blended liquid in polyvinyl alcohol water solution, and had prepared the PNIPAAm/PVA gelatinous fibre by wet spinning, studies show that this fiber has good temperature response performance.But also find simultaneously, because PNIPAAm is at room temperature water-soluble, thereby the gelatinous fibre performance of preparation and unstable [X.Feng, L.chen, L.L.Ju, Y.P.zhao, Proceedings of SPIE, 2007,64231J].
The PNIPAAm/PVA gelatinous fibre is used for artificial-muscle, compare with pH response gelatinous fibre with electric field response, following advantage is arranged: at first, have hydrophilic segment and hydrophobic part in the chemical constitution of PNIPAAm, (Lower critical solution temperature LCST) is 32 ℃ to the lowest critical solution temperature of its aqueous solution.When temperature was lower than 32 ℃, the PNIPAAm macromolecular chain stretches, and was water-soluble with water generation aquation; When temperature was higher than 32 ℃, the PNIPAAm macromolecular chain shrank, and dewaters.PNIPAAm is combined with hydrophilic PVA, can make the lowest critical solution temperature of gelatinous fibre rise to 37 ℃ by regulating the copolymerization ratio, very close with the body temperature of human body, this will bring very big facility for the application of artificial-muscle in human body.Secondly, polyvinyl alcohol (being called for short PVA) has good water-solubility and film forming, and nonpoisonous and tasteless, to the skin nonirritant, is a kind of polymer of green, all uses to some extent at aspects such as medical domain such as ophthalmology, wound dressing, joint prosthesis, artificial kidney films.More valuable is, the PVA aquogel also has advantages such as higher modulus of elasticity and mechanical strength when keeping high water absorption, and this prepares the requirement that artificial-muscle must reach just.
Summary of the invention
At the deficiency of prior art and research, the blank of NIPAAm thermosensitive in situ gel fiber development technology particularly, the present invention proposes preparation method of a kind of temperature sensitive polymer gel fiber material of meter and products thereof.With traditional gel phase ratio, this product has the intensity height, and advantages such as response speed is fast, good biocompatibility have wider application prospect at aspects such as artificial-muscles; The preparation method of this product has controllability well, and technology is simple, and cost is low, does not need characteristics such as special installation and industrializing implementation be easy.
The invention provides a kind of gelatinous fibre with temperature response performance, this gelatinous fibre is that the PNIPAAm/PVA blend is through the wet spinning technology preparation.The mass ratio of NIPAAm and PVA is: 5%-25%.PNIPAAm provides temperature sensitivity, and PVA provides better spinnability energy and bio-compatible performance, and the form of fiber can make product have better mechanical strength and response performance again.
Temperature-sensitive macromolecular gel fiber material preparation method of the present invention comprises the steps:
(1) original position initiated polymerization NIPAAm in the PVA aqueous solution, preparation PNIPAAm/PVA gelatinous fibre spinning solution.Be specially: be 10% PVA with mass concentration 90-100 ℃ deionized water for stirring dissolving 2-5 hour, obtain transparent aqueous solution, naturally cool to room temperature, the adding mass percent is NIPAAm monomer and the initiator ammonium persulfate (APS) of 5%-25% (with respect to PVA), the mass ratio of APS and NIPAAm is (0.005-0.015), add accelerant N again, N, N ', N '-tetramethylethylenediamine (TEMED), the volume ratio of controlling itself and mother liquor is 0.2%-0.3%, mixes 1-2h, feeds N
220-30 minute to drive away oxygen.Above-mentioned mixed solution is sealed in the wide neck flask, and polymerisation 5-7h under 60 ℃ of-70 ℃ of bath temperatures obtains milky PNIPAAm/PVA mixed solution, as spinning solution.
(2) preparation of the nascent polymer gel fiber of PNIPAAm/PVA.Pour above-mentioned spinning solution into spinning machine, water-bath is heated to 90 ℃, and room temperature is clamp-oned in the saturated ammonium sulfate solution that configures, and solidifies typing more than 30 minutes, puts into deionized water and soaks 6-7 days, removes unconverted monomer and some micromolecule.
(3) the nascent gelatinous fibre of vacuum heat PNIPAAm/PVA.With nascent gelatinous fibre air dry at room temperature more than 48 hours, 40-50 ℃ was continued dry 24 hours, vacuumize 24 hours under this temperature then, keep the vacuum condition elevated temperature to continue to dehydrate 1-3 hour to 100-110 ℃, obtain polyvinyl alcohol/poly N-isopropyl acrylamide gel fiber.
Beneficial effect:
The present invention is in the PVA aqueous solution, in-situ polymerization NIPAAm, thereby obtain the PNIPAAm/PVA co-mixing system, utilize PVA better spinnability energy, pass through wet spinning, preparation PNIPAAm/PVA fiber, because the physical entanglement between the hydroxyl on the PVA and the hydrogen bond action of the amino on the NIPAAm and the two kinds of macromolecule molecules, make solution have crosslinked tridimensional network, this fibrous three-dimensional-structure not only can keep gel good water absorption and swelling performance and temperature response performance, but also can effectively improve the intensity of fiber.In order to make the network structure between PVA and the PNIPAAm more stable, further nascent gelatinous fibre is passed through vacuum heat treatment process, to improve its heat resistance.
Compare with thermo-responsive hydro gel, this kind temperature-sensitive macromolecular gel fiber material of the present invention has the intensity height, and response speed is fast, and good biocompatibility to advantage such as the structure of muscle is more similar, will have wide practical use in the artificial-muscle field.PNIPAAm is combined with hydrophilic PVA, can make the LCST of gelatinous fibre rise to 37 ℃ by regulating the ratio of the two, very close with the body temperature of human body, this will bring very big facility for the application of artificial-muscle in human body.Secondly, PVA has good water-solubility and film forming, and nonpoisonous and tasteless, to the skin nonirritant, is a kind of polymer of green, all uses to some extent at aspects such as medical domain such as ophthalmology, wound dressing, joint prosthesis, artificial kidney films.More valuable is, polyvinyl alcohol hydrogel also has advantages such as higher modulus of elasticity and mechanical strength when keeping high water absorption, and this prepares the requirement that artificial-muscle must reach just.In addition, PVA has the better spinnability energy, and its wet spinning technology is also very ripe, and this preparation and performance improvement thereof for gelatinous fibre provides good condition.
In the preparation thermo-sensitive gel fiber preparation method used in the present invention, the method and the wet spinning technology of the in-situ polymerization that uses, be the preparation method of tradition, maturation, technology is simple, just can carry out under atmospheric pressure state, used reagent is conventional reagent, equipment is not also had the particularization requirement, realize industrializing implementation easily, environment is not polluted, preparation cost is cheap, is convenient to promote the use of.The present invention compares than the inventor's early-stage Study, because aquagel fibre is heat-treated, makes that the structure of gelatinous fibre is more stable, and the performance of gelatinous fibre obtains very big improvement.
The specific embodiment
Further narrate the present invention below in conjunction with embodiment:
Below provide specific embodiments of the invention, but the present invention is not subjected to the restriction of specific embodiment.
Embodiment 1:
(1) preparation PNIPAAm/PVA gelatinous fibre spinning solution.With quality is that to be dissolved in the 44ml temperature be in 98 ℃ of deionized waters for the PVA of 4.4g, stirring and dissolving 3 hours, obtain transparent aqueous solution, naturally cool to room temperature, add 1.1g NIPAAm monomer and 0.011g initiator A PS, add promoter TEMED 100 μ l again, mother liquor mixes 1h, feeds N2 bubbling 30 minutes to drive away oxygen.Above-mentioned mixed solution is sealed in the wide neck flask, and polymerisation 7h under 60 ℃ of bath temperatures obtains milky PNIPAAm/PVA mixed solution, as spinning solution.
(2) preparation of the nascent gelatinous fibre of PNIPAAm/PVA macromolecule.Above-mentioned spinning solution is poured in the syringe, and water-bath is heated to 90 ℃, and room temperature is clamp-oned in the saturated ammonium sulfate coagulating bath that configures, and solidifies typing 30 minutes, puts into deionized water and soaks 6 days, removes unconverted monomer and some micromolecule.
(3) PNIPAAm/PVA polymer gel fiber heat treatment.With nascent gelatinous fibre air dry at room temperature more than 48 hours, 40 ℃ were continued dry 24 hours, vacuumize 24 hours under this temperature then keeps vacuum condition elevated temperature to 100 ℃ to continue to dehydrate 1 hour, obtains the PNIPAAm/PVA gelatinous fibre.
Embodiment 2:
(1) preparation PNIPAAm/PVA gelatinous fibre spinning solution.With quality is that to be dissolved in the 44ml temperature be in 98 ℃ of deionized waters for the PVA of 4.4g, stirring and dissolving 3 hours, obtain transparent aqueous solution, naturally cool to room temperature, add 0.88g NIPAAm monomer and 0.0044g initiator A PS, add promoter TEMED90 μ l again, mother liquor mixes 2h, feeds N2 bubbling 30 minutes to drive away oxygen.Above-mentioned mixed solution is sealed in the wide neck flask, and polymerisation 6h under 70 ℃ of bath temperatures obtains milky PNIPAAm/PVA mixed solution, as spinning solution.
(2) preparation of the nascent gelatinous fibre of PNIPAAm/PVA macromolecule.With embodiment 1.
(3) PNIPAAm/PVA polymer gel fiber heat treatment.With nascent gelatinous fibre air dry at room temperature more than 48 hours, 40 ℃ were continued dry 24 hours, vacuumize 24 hours under this temperature then keeps vacuum condition elevated temperature to 100 ℃ to continue to dehydrate 2 hours, obtains the PNIPAAm/PVA gelatinous fibre.
Embodiment 3:
(1) preparation PNIPAAm/PVA gelatinous fibre spinning solution.With quality is that to be dissolved in the 44ml temperature be in 98 ℃ of deionized waters for the PVA of 4.4g, stirring and dissolving 4 hours, obtain transparent aqueous solution, naturally cool to room temperature, add 0.66g NIPAAm monomer and 0.0099g initiator A PS, add promoter TEMED120 μ l again, mother liquor mixes 2h, feeds N2 bubbling 30 minutes to drive away oxygen.Above-mentioned mixed solution is sealed in the wide neck flask, and polymerisation 7h under 65 ℃ of bath temperatures obtains milky PNIPAAm/PVA mixed solution, as spinning solution.
(2) preparation of the nascent gelatinous fibre of PNIPAAm/PVA macromolecule.With embodiment 1.
(3) PNIPAAm/PVA polymer gel fiber heat treatment.With embodiment 2.
Embodiment 4:
(1) preparation PNIPAAm/PVA gelatinous fibre spinning solution.With quality is that to be dissolved in the 44ml temperature be in 98 ℃ of deionized waters for the PVA of 4.4g, stirring and dissolving 3 hours, obtain transparent aqueous solution, naturally cool to room temperature, add 0.44g NIPAAm monomer and 0.0044g initiator A PS, add promoter TEMED100 μ l again, mother liquor mixes 1h, feeds N2 bubbling 30 minutes to drive away oxygen.Above-mentioned mixed solution is sealed in the wide neck flask, and polymerisation 5h under 70 ℃ of bath temperatures obtains milky PNIPAAm/PVA mixed solution, as spinning solution.
(2) preparation of the nascent gelatinous fibre of PNIPAAm/PVA macromolecule.With embodiment 1.
(3) PNIPAAm/PVA polymer gel fiber heat treatment.With embodiment 1.
Embodiment 5:
(1) preparation PNIPAAm/PVA gelatinous fibre spinning solution.With quality is that to be dissolved in the 44ml temperature be in 98 ℃ of deionized waters for the PVA of 4.4g, stirring and dissolving 3 hours, obtain transparent aqueous solution, naturally cool to room temperature, add 0.22g NIPAAm monomer and 0.0030g initiator A PS, add promoter TEMED100 μ l again, mother liquor mixes 1h, feeds N2 bubbling 30 minutes to drive away oxygen.Above-mentioned mixed solution is sealed in the wide neck flask, and polymerisation 5h under 70 ℃ of bath temperatures obtains milky PNIPAAm/PVA mixed solution, as spinning solution.
(2) preparation of the nascent gelatinous fibre of PNIPAAm/PVA macromolecule.With embodiment 1.
(3) PNIPAAm/PVA polymer gel fiber heat treatment.With embodiment 1.
Embodiment 6:
(1) preparation PNIPAAm/PVA gelatinous fibre spinning solution.With quality is that to be dissolved in the 44ml temperature be in 98 ℃ of deionized waters for the PVA of 4.4g, stirring and dissolving 2 hours, obtain transparent aqueous solution, naturally cool to room temperature, add 0.79g NIPAAm monomer and 0.0012g initiator A PS, add promoter TEMED100 μ l again, mother liquor mixes 1h, feeds N2 bubbling 30 minutes to drive away oxygen.Above-mentioned mixed solution is sealed in the wide neck flask, and polymerisation 6h under 60 ℃ of bath temperatures obtains milky PNIPAAm/PVA mixed solution, as spinning solution.
(2) preparation of the nascent gelatinous fibre of PNIPAAm/PVA macromolecule.With embodiment 1.
(3) PNIPAAm/PVA polymer gel fiber heat treatment.With embodiment 2.
Embodiment 7:
(1) preparation PNIPAAm/PVA gelatinous fibre spinning solution.With quality is that to be dissolved in the 44ml temperature be in 100 ℃ of deionized waters for the PVA of 4.4g, stirring and dissolving 2 hours, obtain transparent aqueous solution, naturally cool to room temperature, add 0.79g NIPAAm monomer and 0.0012g initiator A PS, add promoter TEMED100 μ l again, mother liquor mixes 1h, feeds N2 bubbling 30 minutes to drive away oxygen.Above-mentioned mixed solution is sealed in the wide neck flask, and polymerisation 6h under 60 ℃ of bath temperatures obtains milky PNIPAAm/PVA mixed solution, as spinning solution.
(2) preparation of the nascent gelatinous fibre of PNIPAAm/PVA macromolecule.With embodiment 1.
(3) PNIPAAm/PVA polymer gel fiber heat treatment.With nascent gelatinous fibre air dry at room temperature more than 48 hours, 45 ℃ were continued dry 24 hours, vacuumize 24 hours under this temperature then keeps vacuum condition elevated temperature to 110 ℃ to continue to dehydrate 2 hours, obtains the PNIPAAm/PVA gelatinous fibre.
Embodiment 8:
(1) preparation PNIPAAm/PVA gelatinous fibre spinning solution.With quality is that to be dissolved in the 44ml temperature be in 100 ℃ of deionized waters for the PVA of 4.4g, stirring and dissolving 2 hours, obtain transparent aqueous solution, naturally cool to room temperature, add 0.79g NIPAAm monomer and 0.0012g initiator A PS, add promoter TEMED100 μ l again, mother liquor mixes 1h, feeds N2 bubbling 30 minutes to drive away oxygen.Above-mentioned mixed solution is sealed in the wide neck flask, and polymerisation 7h under 65 ℃ of bath temperatures obtains milky PNIPAAm/PVA mixed solution, as spinning solution.
(2) preparation of the nascent gelatinous fibre of PNIPAAm/PVA macromolecule.With embodiment 1.
(3) PNIPAAm/PVA polymer gel fiber heat treatment.With nascent gelatinous fibre air dry at room temperature more than 48 hours, 50 ℃ were continued dry 24 hours, vacuumize 24 hours under this temperature then keeps vacuum condition elevated temperature to 100 ℃ to continue to dehydrate 2 hours, obtains the PNIPAAm/PVA gelatinous fibre.
Embodiment 9:
(1) preparation of the nascent gelatinous fibre of PNIPAAm/PVA macromolecule.With embodiment 2.
(2) PNIPAAm/PVA polymer gel fiber heat treatment.With embodiment 2.
(3) PNIPAAm/PVA polymer gel fiber heat treatment.More than 48 hours, 45 ℃ were continued dry 24 hours with nascent gelatinous fibre air dry at room temperature, and vacuumize 24 hours under this temperature then keeps vacuum condition elevated temperature to 105 ℃ outer continuous dehydrating 2 hours, obtains PNIPAAm/PVA.
Claims (4)
1. one kind is used for polymer gel fiber material artificial-muscle, that have temperature response performance, this fiber is that polyvinyl alcohol and poly-N-isopropyl acrylamide blend make through wet spinning technology and heat treatment process, and the mass percent of N-N-isopropylacrylamide and polyvinyl alcohol is 5%-25%.
2. one kind has the preparation method of the polymer gel fiber material of temperature response performance as claim 1, comprises the steps:
(1) original position initiated polymerization N-N-isopropylacrylamide in polyvinyl alcohol water solution, preparation poly-N-isopropyl acrylamide/polyvinyl alcohol gel fiber spinning dope, be specially: be 10% polyvinyl alcohol with mass concentration 90-100 ℃ deionized water for stirring dissolving 2-5 hour, obtain transparent aqueous solution, naturally cool to room temperature, the adding mass percent is N-N-isopropylacrylamide monomer and the initiator ammonium persulfate of 5%-25% (with respect to polyvinyl alcohol), the mass ratio of ammonium persulfate and N-N-isopropylacrylamide is (0.005-0.015), add accelerant N again, N, N ', N '-tetramethylethylenediamine, the volume ratio of controlling itself and mother liquor is 0.2%-0.3%, mixes 1-2h, feeds N2 bubbling 20-30 minute to drive away oxygen.Above-mentioned mixed solution is sealed in the wide neck flask, and polymerisation 5h-7h under 60 ℃ of-70 ℃ of bath temperatures obtains milky polyvinyl alcohol/poly-N-isopropyl acrylamide mixed solution, as spinning solution;
(2) preparation of the nascent polymer gel fiber of poly-N-isopropyl acrylamide/polyvinyl alcohol, above-mentioned spinning solution is poured in the spinning machine, water-bath is heated to 90 ℃, room temperature is clamp-oned in the saturated ammonium sulfate coagulating bath that configures, solidify typing more than 30 minutes, put into deionized water and soaked 6-7 days, remove unconverted monomer and some micromolecule;
(3) the nascent gelatinous fibre of vacuum heat poly-N-isopropyl acrylamide/polyvinyl alcohol, with nascent gelatinous fibre air dry at room temperature more than 48 hours, 40-50 ℃ was continued dry 24 hours, vacuumize 24 hours under this temperature then, keep the vacuum condition elevated temperature to continue to dehydrate 1-3 hour to 100-110 ℃, obtain poly-N-isopropyl acrylamide/polyvinyl alcohol gel fiber.
3. the preparation method of polymer gel fiber according to claim 2, the mass percent of N-N-isopropylacrylamide and polyvinyl alcohol is 5%-25%.
4. a polymer gel fiber material is characterized in that this polymer gel fiber material adopts the described preparation method of claim 2 to make.
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| CN108998960A (en) * | 2018-09-13 | 2018-12-14 | 天津工业大学 | A kind of method that temperature-sensitive nano-gel microballoon arranges pure cotton fabric |
| CN109385692A (en) * | 2018-10-25 | 2019-02-26 | 东华大学 | A kind of thermal actuation hydrogel bundles of nanofibers and its serialization preparation and application |
| CN109385692B (en) * | 2018-10-25 | 2021-09-21 | 东华大学 | Thermal-actuated hydrogel nanofiber bundle and continuous preparation and application thereof |
| CN111455564A (en) * | 2019-01-20 | 2020-07-28 | 泽塔纳米科技（苏州）有限公司 | Antibacterial hydrophilic nanofiber membrane and preparation method thereof |
| CN111690156A (en) * | 2020-06-24 | 2020-09-22 | 王萌燕 | Super-absorbent polymer, super-absorbent gel and preparation method thereof |
| CN115216852A (en) * | 2021-04-15 | 2022-10-21 | 财团法人纺织产业综合研究所 | Temperature-sensing humidity-adjusting fiber and preparation method thereof |
| CN116059440A (en) * | 2023-02-14 | 2023-05-05 | 厦门大学 | Bionic muscle material with anisotropy and preparation method thereof |
| CN116059440B (en) * | 2023-02-14 | 2023-12-19 | 厦门大学 | Bionic muscle material with anisotropy and preparation method thereof |
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