CN109355725A - A kind of preparation method of self-healing property aquagel fibre - Google Patents
A kind of preparation method of self-healing property aquagel fibre Download PDFInfo
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- CN109355725A CN109355725A CN201810969418.1A CN201810969418A CN109355725A CN 109355725 A CN109355725 A CN 109355725A CN 201810969418 A CN201810969418 A CN 201810969418A CN 109355725 A CN109355725 A CN 109355725A
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- polyvinyl alcohol
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- 239000000835 fiber Substances 0.000 title claims abstract description 52
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 35
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 33
- 238000004132 cross linking Methods 0.000 claims abstract description 23
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 11
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 32
- 229940068984 polyvinyl alcohol Drugs 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- -1 polyethylene Polymers 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004698 Polyethylene Substances 0.000 claims description 5
- 238000007605 air drying Methods 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 230000008014 freezing Effects 0.000 claims description 5
- 238000007710 freezing Methods 0.000 claims description 5
- 239000008236 heating water Substances 0.000 claims description 5
- 238000002513 implantation Methods 0.000 claims description 5
- 229920000573 polyethylene Polymers 0.000 claims description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- 235000019394 potassium persulphate Nutrition 0.000 claims description 5
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 238000006136 alcoholysis reaction Methods 0.000 claims description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 2
- 150000001408 amides Chemical class 0.000 claims 1
- 239000000017 hydrogel Substances 0.000 abstract description 22
- 238000000034 method Methods 0.000 abstract description 18
- 239000000463 material Substances 0.000 abstract description 9
- 238000010382 chemical cross-linking Methods 0.000 abstract description 4
- 239000004744 fabric Substances 0.000 abstract description 3
- 239000000178 monomer Substances 0.000 abstract description 2
- 238000002166 wet spinning Methods 0.000 abstract description 2
- 239000003999 initiator Substances 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 239000003431 cross linking reagent Substances 0.000 description 5
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 238000011069 regeneration method Methods 0.000 description 5
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 4
- 239000000499 gel Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- 230000006378 damage Effects 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 1
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000009120 camo Nutrition 0.000 description 1
- 235000005607 chanvre indien Nutrition 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 229920006037 cross link polymer Polymers 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000011487 hemp Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000003032 molecular docking Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229920003169 water-soluble polymer Polymers 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F261/00—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00
- C08F261/02—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols
- C08F261/04—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols on to polymers of vinyl alcohol
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/243—Two or more independent types of crosslinking for one or more polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The present invention relates to intellectual material fields, disclose a kind of preparation method of self-healing property aquagel fibre.This method are as follows: using polyvinyl alcohol, acrylamide, acrylic acid as monomer, the hydrogel with self-repairing capability is obtained by the way of chemical crosslinking and with physical crosslinking, conductive aquagel fibre is obtained using the method for wet spinning, hydrogel also has preferable toughness simultaneously, and flexibility, it can be woven into fiber cloth, it can also be with other fiber shufflings at various function fabrics.
Description
Technical field
The present invention relates to intellectual material field more particularly to a kind of preparation methods of self-healing property aquagel fibre.
Background technique
Hydrogel (Hydrogel) is the gel using water as decentralized medium.Water soluble polymer with cross-linked network
It is middle to introduce a part of hydrophobic grouping and hydrophilic residue, hydrophilic residue and water molecules, hydrone is connected to netted inside, and
The cross-linked polymer of hydrophobic residue water-swellable.It is a kind of macromolecule network system, property is soft, it is able to maintain certain shape,
A large amount of water can be absorbed.PVA hydrogel has good non-toxic and biocompatibility, can be applied in daily life, very
To be applied to biomedicine in.
Usually there is the disadvantages of gel strength is low, poor toughness and absorption speed are slow in hydrogel, be unable to satisfy the requirement used.
So reinforcing the workability of hydrogel come mechanical performances such as strength and toughnesses for enhancing hydrogel by the way of crosslinking, open up
The use scope of hydrogel is opened up, the mode of crosslinking can be divided into physical crosslinking and chemical crosslinking two major classes.And be only physical crosslinking or
Chemical crosslinking cannot all obtain the hydrogel of rationality intensity, so double cross-linking patterns have been included into the design thinking range of hydrogel
It is interior.
Fiber applications are extensive, can be made into filament, the end of a thread and the rope made of hemp, and papermaking or while knitting felt can also be made into fibrous layer；Simultaneously
Also it is commonly used to manufacture unclassified stores, and collectively constitutes composite material with unclassified stores, there is great purposes in human lives,
The use of fiber generally requires fiber and has certain intensity, and the hydrogel for passing through double cross connection can be competent at this " fabric ".
The self-reparing capability of material is broadly divided into two major classes, and the selfreparing of foreign aid's property and intrinsic selfreparing, foreign aid's property are reviewed one's lessons by oneself
It is repairing monomer or adhesive and realize selfreparing by material package again, repairing performance is limited.So we gradually will
Sight shifts to intrinsic self-repair material.Wish what self-repair material itself can be received by the special role self-regeneration of itself
Damage.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of preparation methods of self-healing property aquagel fibre.This hair
In bright method, using the water-setting with very good mechanical properties of the physical-chemical double cross linked method preparation of the method for the present invention preparation
Glue fiber, intensity, toughness with higher, high transparency, it is more standby be cut off after self-reparing capability, improve material
Durability.The present invention uses process for copolymerization, realizes chemical crosslinking, then the method for taking repeatedly freeze-thaw makes water
There is crystallite area inside gel, realizes physical crosslinking.Had using the aquagel fibre of the method for the present invention preparation good
Mechanical performance, high transparency, self-regeneration.
The specific technical proposal of the invention is: a kind of preparation method of self-healing property aquagel fibre, comprising the following steps:
Step 1), polyethylene dissolving alcohol: polyvinyl alcohol is added in deionized water, heating water bath is to 70-80 DEG C, by acutely stirring
Mixing dissolves polyvinyl alcohol, is then allowed to stand after polyvinyl alcohol is completely dissolved, and obtains poly-vinyl alcohol solution, for use.
Polyvinyl alcohol is due to having certain degree of polymerization, so needing under conditions of certain liter gentle agitation, promotes
Solvent molecule is spread into polymer, and polyvinyl alcohol is allowed to be swollen and dissolve.
Acrylamide and acrylic acid are added into poly-vinyl alcohol solution by step 2), in mass ratio (40:60)-(30:70), stir
It mixes uniformly, ultrasonic disperse, for use.
Potassium peroxydisulfate is added by 600-700mg/ml and presses solution gross mass 1.5-2.5% addition N, N- methylene for step 3)
Bisacrylamide.
It joined crosslinking agent when reaction, so that obtained polymer has certain chemical bond degree of cross linking, have certain strong
Degree.Reaction time is unsuitable too short or too long, and the reaction time, the too short degree of polymerization was not high, and the condition of fiber applications is not achieved in intensity, and
Reaction time can not be too long, and reaction time too long meeting can not become so that the right high and excessively high degree of cross linking of polymer poly
Spinning solution carries out wet spinning, or has carried out spinning but fiber can really up to the mark in time, does not have flexibility or fiber is firmly crisp easily broken.
Step 4) pours into step 3) acquired solution in three-neck flask, and logical nitrogen is caught up with except oxygen, causes at 55-65 DEG C
Acrylamide and acrylic acid are copolymerized conjunction, reaction time 4-6h；
Step 5), using syringe by reaction solution implantation quality score be 1-3% sodium hydrate aqueous solution in solidificating fiber,
Natural air drying is taken out after placing 4-8h, obtains aquagel fibre；
Step 6), to after completion of the reaction, aquagel fibre be freezed 3-5h at -80 DEG C to -60 DEG C, take out, solve at room temperature
Freeze 10-14h, thaw after freezing 6h at -80 to -60 DEG C, reciprocal 3 times, forms crystallite area point physical crosslinking, finally obtain certainly
More property aquagel fibre.
In the prior art, compare the method for lacking and hydrogel being prepared as fiber, be primarily due to conventional hydrogels intensity,
Toughness is poor, less meets the application positioning of fiber.And the present invention greatly improves hydrogel using the method for double cross connection
Mechanical performance, so that aquagel fibre is prepared into for reality.And containing a large amount of in prepared by the method hydrogel
Hydrogen bond realize the self-regeneration of aquagel fibre.
In the methods of the invention, using N, N- methylene-bisacrylamide makes polymer molecule be cross-linked with each other, and uses
The method of freeze-thaw repeatedly forms crystallite area node between polyvinyl alcohol molecule, polymer molecule is allowed to be linked to be net
Network structure forms physics cross-linked structure, greatly enhances the performance of crosslinking, enhance the mechanical performance of fiber, and physics
The dynamic reversible characteristic of cross-linked network enables hydrogel to carry out selfreparing under the harsh conditions of general non-cryogenic.Conductive water-setting
Its fracture port can be carried out docking and carry out selfreparing, the fibre after reparation by glue fiber when fracture having occurred when applying as conducting wire
Dimension still has certain mechanical strength and electric conductivity, it is not necessary to change and substitute circuit.
In the present invention, fiber flexibility, toughness, preferable intensity, electrically conductive, transparent and self-regeneration performance.
Preferably, in step 1), the M of the polyvinyl alcoholw=89000-98000, percent alcoholysis > 99%.
Preferably, in step 1), mixing time 1-3h.
Preferably, the ultrasonic disperse time is 20-40min in step 2), ultrasonic 5min suspends 3min.
Ultrasonic disperse wants ultrasonic 5min pause 3min, avoids heat accumulation when ultrasound, is surpassed before initiator is added
Sound dispersion, can only carry out mechanical stirring after adding initiator and crosslinking agent, inevitable heat production when ultrasound is avoided to send out
Raw premature polymerization.Polymerization reaction will have free radical just to can be carried out, and then cause chain reaction, polymerization inhibitor meeting of the oxygen as reaction
(free radical attack oxygen-oxygen bond forms the intermediate of similar peroxide) is quenched in the free radical made, thus prevent reaction continue into
Row, not can be carried out polymerization or needs using more initiators.
Preferably, carrying out rousing nitrogen 30min to solution before reaction, driving the oxygen incorporated in solution out of in step 4).
The copolymer chain that free radical polymerization generates mutually is tangled by intermolecular hydrogen bonding effect, forms physical crosslinking
Crosslinking points.This is one of physical crosslinking physical crosslinking point.It is polyvinyl alcohol in low temperature cold repeatedly there are also a kind of crosslinking points
Freeze and make polyvinyl alcohol chain generate certain orientation during thawing, and form the cross-linked microcrystalline area of physics, forms crosslinking
Network.
It is compared with the prior art, the beneficial effects of the present invention are:
1, the method for the present invention selects polyvinyl alcohol as raw material, and having good non-toxic and biocompatibility is as fiber
Excellent selection.
2, the aquagel fibre of the method for the present invention preparation has excellent mechanical performance, is that conventional hydrogels material cannot
It realizes, by way of being chemically crosslinked and being physical crosslinking two kinds of crosslinking methods and deposit hydrogel has been reached and be prepared into fiber
Condition.
3, preparation process of the present invention is simple, environmental-friendly, energy-efficient, and gained conductive fiber is contained abundant by itself
Strong hydrogen bonding be provided with self-repairing capability, strengthen the injury resistant ability of material, conductive fiber breakage need not substitute, directly will
Fracture, which contacts with each other, may wait for self-regeneration.
Specific embodiment
The present invention will be further described with reference to the examples below.
Embodiment 1:
Step 1: polyethylene dissolving alcohol: polyvinyl alcohol 1.2g being added in 6.8ml deionized water, is placed in water-bath environment
Heating water bath is carried out to 75 DEG C, by being vigorously stirred stirring 2h polyvinyl alcohol is dissolved in deionized water, is then allowed to stand
Polyvinyl alcohol to be confirmed is stand-by after being completely dissolved.
Step 2: 0.85g acrylamide and 1.85g propylene is added in polyvinyl alcohol uniform solution obtained in step 1
Acid is uniformly dispersed in the two in the poly-vinyl alcohol solution with certain viscosity by churned mechanically effect, ultrasound
Disperse 40min, ultrasonic 5min suspends 3min, for use.
Step 3: in two solution of above-mentioned steps be added potassium peroxydisulfate (650mg/ml) as reaction carry out initiator and
The crosslinking agent that the N,N methylene bis acrylamide of 55.6mg is chemically crosslinked as hydrogel.
Step 4: solution made from step 3 is poured into bottle, logical nitrogen is caught up with except oxygen, causes acrylamide at 60 DEG C
Conjunction, reaction time 4h are copolymerized with acrylic acid.
Step 5: being frozen into the sodium hydrate aqueous solution for the use of syringe being 2% by reaction solution implantation quality score
Fiber takes out natural air drying after 6h to be placed.
Step 6: aquagel fibre is placed in low temperature refrigerator to after completion of the reaction, 4h is freezed under the conditions of -70 DEG C, is taken
Out, thaw 12h at room temperature, then is placed in refrigerator and thaws after freezing 6h, reciprocal 3 times, can form crystallite area point physical crosslinking, most
The aquagel fibre that chemical-physical double cross connection has self-healing property is obtained eventually.
Embodiment 2:
Step 1: polyethylene dissolving alcohol: polyvinyl alcohol 1.2g being added in 6.8ml deionized water, is placed in water-bath environment
Heating water bath is carried out to 75 DEG C, by being vigorously stirred stirring 2h polyvinyl alcohol is dissolved in deionized water, is then allowed to stand
Polyvinyl alcohol to be confirmed is stand-by after being completely dissolved.
Step 2: 0.992g acrylamide and 1.668g third is added in polyvinyl alcohol uniform solution obtained in step 1
Olefin(e) acid is uniformly dispersed in the two in the poly-vinyl alcohol solution with certain viscosity by churned mechanically effect, surpasses
Sound disperses 20min, and ultrasonic 5min suspends 3min, for use.
Step 3: in two solution of above-mentioned steps be added potassium peroxydisulfate (650mg/ml) as reaction carry out initiator and
The crosslinking agent that the N,N methylene bis acrylamide of 55.6mg is chemically crosslinked as hydrogel；
Step 4: solution made from step 3 is poured into bottle, logical nitrogen is caught up with except oxygen, causes acrylamide and third at 60 DEG C
Olefin(e) acid is copolymerized conjunction, reaction time 5h.
Step 5: being frozen into the sodium hydrate aqueous solution for the use of syringe being 2% by reaction solution implantation quality score
Fiber takes out natural air drying after 6h to be placed.
Step 6: aquagel fibre is placed in low temperature refrigerator to after completion of the reaction, 4h is freezed under the conditions of -70 DEG C, is taken
Out, thaw 12h at room temperature, then is placed in refrigerator and thaws after freezing 6h, reciprocal 3 times, can form crystallite area point physical crosslinking, most
The aquagel fibre that chemical-physical double cross connection has self-healing property is obtained eventually.
Embodiment 3:
Step 1: polyethylene dissolving alcohol: polyvinyl alcohol 1.2g being added in 6.8ml deionized water, is placed in water-bath environment
Heating water bath is carried out to 75 DEG C, by being vigorously stirred stirring 2h polyvinyl alcohol is dissolved in deionized water, is then allowed to stand
Polyvinyl alcohol to be confirmed is stand-by after being completely dissolved.
Step 2: 0.834g acrylamide and 1.946g third is added in polyvinyl alcohol uniform solution obtained in step 1
Olefin(e) acid is uniformly dispersed in the two in the poly-vinyl alcohol solution with certain viscosity by churned mechanically effect, surpasses
Sound disperses 30min, and ultrasonic 5min suspends 3min, for use.
Step 3: in above-mentioned steps two) initiator of potassium peroxydisulfate (650mg/ml) as reaction progress is added in solution
The crosslinking agent being chemically crosslinked with the N,N methylene bis acrylamide of 55.6mg as hydrogel；
Step 4: solution made from step 3 is poured into bottle, logical nitrogen is caught up with except oxygen, causes acrylamide and third at 60 DEG C
Olefin(e) acid is copolymerized conjunction, reaction time 6h.
Step 5: being frozen into the sodium hydrate aqueous solution for the use of syringe being 2% by reaction solution implantation quality score
Fiber takes out natural air drying after 6h to be placed.
Step 6: aquagel fibre is placed in low temperature refrigerator to after completion of the reaction, 4h is freezed under the conditions of -70 DEG C, is taken
Out, thaw 12h at room temperature, then is placed in refrigerator and thaws after freezing 6h, reciprocal 3 times, can form crystallite area point physical crosslinking, most
The aquagel fibre that chemical-physical double cross connection has self-healing property is obtained eventually.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field；In the present invention
Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention
Technical spirit any simple modification, change and equivalent transformation to the above embodiments, still fall within the technology of the present invention side
The protection scope of case.
Claims (5)
1. a kind of preparation method of self-healing property aquagel fibre, it is characterised in that the following steps are included:
Step 1), polyethylene dissolving alcohol: polyvinyl alcohol is added in deionized water, heating water bath is to 70-80 DEG C, by acutely stirring
Mixing dissolves polyvinyl alcohol, is then allowed to stand after polyvinyl alcohol is completely dissolved, and obtains poly-vinyl alcohol solution, for use；
Acrylamide and acrylic acid are added into poly-vinyl alcohol solution by step 2), in mass ratio (40:60)-(30:70), and stirring is equal
It is even, ultrasonic disperse, for use；
Potassium peroxydisulfate is added by 600-700mg/ml and presses solution gross mass 1.5-2.5% addition N, N- di-2-ethylhexylphosphine oxide third for step 3)
Acrylamide；
Step 4) pours into step 3) acquired solution in three-neck flask, and logical nitrogen is caught up with except oxygen, causes propylene at 55-65 DEG C
Amide and acrylic acid are copolymerized conjunction, reaction time 4-6h；
Step 5), using syringe by reaction solution implantation quality score be 1-3% sodium hydrate aqueous solution in solidificating fiber,
Natural air drying is taken out after placing 4-8h, obtains aquagel fibre；
Step 6), to after completion of the reaction, aquagel fibre be freezed 3-5h at -80 DEG C to -60 DEG C, take out, solve at room temperature
Freeze 10-14h, thaw after freezing 6h at -80 to -60 DEG C, reciprocal 3 times, forms crystallite area point physical crosslinking, finally obtain certainly
More property aquagel fibre.
2. a kind of preparation method of self-healing property aquagel fibre as described in claim 1, which is characterized in that in step 1), institute
State the M of polyvinyl alcoholw=89000-98000, percent alcoholysis > 99%.
3. a kind of preparation method of self-healing property aquagel fibre as described in claim 1, which is characterized in that in step 1), stir
Mixing the time is 1-3h.
4. a kind of preparation method of self-healing property aquagel fibre as described in claim 1, which is characterized in that in step 2), surpass
Sound jitter time is 20-40min, and ultrasonic 5min suspends 3min.
5. a kind of preparation method of self-healing property aquagel fibre as described in claim 1, which is characterized in that in step 4), instead
Solution is carried out before answering to rouse nitrogen 30min, drives the oxygen incorporated in solution out of.
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| WO2021046930A1 (en) * | 2019-09-10 | 2021-03-18 | 华南理工大学 | High-transparency self-healing solid material, preparation method therefor, and application thereof |
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| CN114539487A (en) * | 2022-03-25 | 2022-05-27 | 深圳市华星光电半导体显示技术有限公司 | Conductive material, electronic device and manufacturing method thereof |
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| CN114606594A (en) * | 2022-03-08 | 2022-06-10 | 东华大学 | Stretchable and elastic conductive polymer-based hydrogel fiber and preparation method thereof |
| CN114539487A (en) * | 2022-03-25 | 2022-05-27 | 深圳市华星光电半导体显示技术有限公司 | Conductive material, electronic device and manufacturing method thereof |
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