CN106381570B - A kind of electrospinning nylon 46/PVA/ boric acid composite nano fibers and preparation method thereof - Google Patents
A kind of electrospinning nylon 46/PVA/ boric acid composite nano fibers and preparation method thereof Download PDFInfo
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- CN106381570B CN106381570B CN201610846668.7A CN201610846668A CN106381570B CN 106381570 B CN106381570 B CN 106381570B CN 201610846668 A CN201610846668 A CN 201610846668A CN 106381570 B CN106381570 B CN 106381570B
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- boric acid
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- 239000004327 boric acid Substances 0.000 title claims abstract description 125
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 239000002121 nanofiber Substances 0.000 title claims abstract description 65
- 229920003189 Nylon 4,6 Polymers 0.000 title claims abstract description 58
- 239000002131 composite material Substances 0.000 title claims abstract description 57
- 238000001523 electrospinning Methods 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims description 18
- SHPVGWLRFPFLNE-UHFFFAOYSA-N butane-1,4-diamine;hexanedioic acid Chemical compound NCCCCN.OC(=O)CCCCC(O)=O SHPVGWLRFPFLNE-UHFFFAOYSA-N 0.000 claims abstract description 84
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 230000010070 molecular adhesion Effects 0.000 claims abstract description 8
- 239000000654 additive Substances 0.000 claims abstract description 7
- 230000000996 additive effect Effects 0.000 claims abstract description 7
- 125000005619 boric acid group Chemical group 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 38
- 239000011259 mixed solution Substances 0.000 claims description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 238000010041 electrostatic spinning Methods 0.000 claims description 25
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 24
- 239000002243 precursor Substances 0.000 claims description 21
- 150000003839 salts Chemical class 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- 239000004745 nonwoven fabric Substances 0.000 claims 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 141
- 229920002451 polyvinyl alcohol Polymers 0.000 description 141
- 239000004677 Nylon Substances 0.000 description 25
- 229920001778 nylon Polymers 0.000 description 25
- 238000009987 spinning Methods 0.000 description 24
- 239000000835 fiber Substances 0.000 description 16
- 239000000463 material Substances 0.000 description 14
- 229920000642 polymer Polymers 0.000 description 14
- 239000000523 sample Substances 0.000 description 12
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 9
- 229910052796 boron Inorganic materials 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 8
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 239000004744 fabric Substances 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 229920001577 copolymer Polymers 0.000 description 5
- 239000000178 monomer Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 4
- 229920002302 Nylon 6,6 Polymers 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 235000019253 formic acid Nutrition 0.000 description 4
- 229920006324 polyoxymethylene Polymers 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 229920006351 engineering plastic Polymers 0.000 description 3
- 238000005227 gel permeation chromatography Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000004166 bioassay Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000003502 gasoline Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 229920001897 terpolymer Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical class CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000004425 Makrolon Substances 0.000 description 1
- 241000549556 Nanos Species 0.000 description 1
- 229920001207 Noryl Polymers 0.000 description 1
- 239000004727 Noryl Substances 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- -1 Polybutylene terephthalate Polymers 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 150000001241 acetals Chemical class 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 125000000914 phenoxymethylpenicillanyl group Chemical group CC1(S[C@H]2N([C@H]1C(=O)*)C([C@H]2NC(COC2=CC=CC=C2)=O)=O)C 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920005594 polymer fiber Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001007 puffing effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
Abstract
The present invention provides a kind of electrospinning nylon 46/PVA/ boric acid composite nano fibers, and the composite nano fiber includes nylon 46 salt, molecular adhesion agent and heat-resisting additive, wherein the molecular adhesion agent is PVA, and the heat-resisting additive is boric acid；The mass ratio of the nylon 46 salt and the PVA are (0.4~6)：1.
Description
Technical field
The invention belongs to polymeric material fields, more particularly it relates to which a kind of electrospinning nylon 46/PVA/ boric acid is multiple
Close nanofiber and preparation method thereof.
Background technology
With the rapid development of science and technology, variation with rapid changepl. never-ending changes and improvements is just occurring for material science.It is metal material, inorganic non-
Metal material, high molecular material and composite material have become four big stay materials of the world today, high molecular material, with its chemistry
The advantages that stability is good, light weight, good insulating, more forming method and be widely used in industry now and daily life production,
Wherein engineering plastics have many advantages, such as density is small, intensity is high, excellent hot property, electrical property and chemical resistance with it,
As one of the essential new material in new high-tech industry.Nylon, makrolon, polyformaldehyde, Noryl and
Polybutylene terephthalate is frequently referred to five large-engineering plastics.
Currently, the technology for preparing nanosized polymer fiber by electrostatic spinning is increasingly mature, and nano grade polymer is fine
Dimension due to very big major diameter when recuperability, and to material mechanical performance and hot property have significant raising
Effect.The large-scale production of nanofiber industrially provides possibility to expand its application industrially.Nylon is due to it
The feature that nanofiber diameter is small, toughness and intensity are high is all applied to day as a kind of good spinning material all the time
Often in life.Nylon is only soluble in a small number of solvents such as formic acid, dimethyl sulfoxide (DMSO), and the smell of formic acid is big and toxic, is not suitable for big rule
The electrospinning of modelling prepares nylon nano fiber.
In view of the above-mentioned problems, existing, there is an urgent need for electrospinnings in a kind of safety of exploitation, lower-cost aqueous solution to prepare toughness and intensity
The technology of high nylon composite nano-fiber material.
Invention content
To solve the above-mentioned problems, one aspect of the present invention provides a kind of electrospinning nylon 46/PVA/ boric acid composite Nanos
Fiber, the composite nano fiber include nylon 46 salt, molecular adhesion agent and heat-resisting additive, wherein the molecular adhesion agent
For PVA, the heat-resisting additive is boric acid；The mass ratio of the nylon 46 salt and the PVA are (0.4~6)：1.
In one embodiment, the mass ratio of the PVA and the boric acid is (1~6)：1.
In one embodiment, the mass ratio of the PVA and the boric acid is (1~5)：1.
In one embodiment, the weight average molecular weight of the PVA is 1.6 × 104~1 × 105g/mol。
Another aspect of the present invention provides a kind of preparation method of electrospinning nylon 46/PVA/ boric acid composite nano fibers, packet
Include following steps：
(1) sample dissolves：Nylon 46 salt is dissolved in deionized water；
(2) raw material mixes：PVA, boric acid are added in step (1) solution in mass ratio, stirred, is uniformly mixed, obtains
To nylon 46 salt/PVA/ boric acid mixed solutions；
(3) electrostatic spinning：The step (2) nylon 46 salt/PVA/ boric acid mixed solutions are prepared into nylon by electrospinning
46 salt/PVA/ boric acid precursor；
(4) it is heat-treated：The step (3) nylon 46 salt/PVA/ boric acid mixed solutions are prepared into nylon 46 salt/PVA/ boron
Sour precursor is dried, and after heat treatment, obtains the nylon 46/PVA/ boric acid composite nano fibers.
In one embodiment, nylon 46 salt and the mass ratio of the deionized water described in the step (1) are
(0.3~0.5)：1.
In one embodiment, drying temperature described in the step (4) be 80~100 DEG C, drying time be 1.0~
2.0h。
In one embodiment, heat treatment temperature described in the step (4) is 180~300 DEG C, and heat treatment time is
0.5~2h.
In one embodiment, a diameter of 10~400nm of the nylon 46/PVA/ boric acid composite nano fibers.
In one embodiment, the electrospinning nylon 46/PVA/ boric acid composite nano fibers are applied to non-woven cloth collar
Domain.
The above-mentioned of the application and other features, aspect and advantage is more readily understood with reference to following detailed description.
Specific implementation mode
The detailed description for preferred implementation method of the invention below of participating in the election of and including embodiment this hair can be more easily understood
Bright content.Unless otherwise defined, all technologies used herein and scientific terminology have common with fields of the present invention
The normally understood identical meaning of technical staff.When there is a conflict, the definition in this specification shall prevail.
As used herein term " by ... prepare " it is synonymous with "comprising".Term "comprising" used herein, " comprising ",
" having ", " containing " or its any other deformation, it is intended that cover non-exclusionism includes.For example, the combination comprising listed elements
Object, step, method, product or device are not necessarily limited to those elements, but may include not expressly listed other elements or
Such composition, step, method, product or the intrinsic element of device.
Conjunction " Consists of " excludes any element that do not point out, step or component.If in claim, this
Phrase will make claim be closed, so that it is not included the material in addition to the material of those descriptions, but relative normal
Except rule impurity.When being rather than immediately following after theme in the clause that phrase " Consists of " appears in claim main body,
It is only limited to the element described in the clause；Other elements are not excluded except the claim as a whole.
Equivalent, concentration or other values or parameter are excellent with range, preferred scope or a series of upper limit preferred values and lower limit
When the Range Representation that choosing value limits, this, which should be understood as, specifically discloses by any range limit or preferred value and any range
Any pairing of lower limit or preferred value is formed by all ranges, regardless of whether the range separately discloses.For example, when open
When range " 1 to 5 ", described range should be interpreted as including range " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to
5 ", " 1 to 3 and 5 " etc..When numberical range is described herein, unless otherwise stated, otherwise range intention includes its end
Value and all integers and score in the range.
Singulative includes that plural number discusses object, unless the context clearly dictates otherwise." optional " or it is " arbitrary
It is a kind of " refer to that the item described thereafter or event may or may not occur, and the description include situation that event occurs and
The situation that event does not occur.
Approximate term in specification and claims is used for modifying quantity, and it is specific to indicate that the present invention is not limited to this
Quantity further includes the modified part of the acceptable change without lead to related basic function close to the quantity.Phase
It answers, modifies a numerical value with " about ", " about " etc., mean that the present invention is not limited to the exact numericals.In some examples, approximate
Term likely corresponds to the precision of the instrument of measured value.In present specification and claims, range limits can be with
Combination and/or exchange, these ranges include all subranges contained therebetween if not stated otherwise.
In addition, indefinite article "an" before element of the present invention or component and "one" quantitative requirement to element or component
(i.e. occurrence number) unrestriction.Therefore "one" or "an" should be read as including one or at least one, and odd number
The element or component of form also include plural form, unless the apparent purport of the quantity refers to singulative.
" polymer " means the polymerizable compound prepared by the monomer by the identical or different type of polymerization.Generic term
" polymer " includes term " homopolymer ", " copolymer ", " terpolymer " and " copolymer ".
" copolymer " means the polymer prepared by polymerizeing at least two different monomers.Generic term " copolymer " includes
(it is general with term " terpolymer " for term " copolymer " (its generally to refer to the polymer prepared by two kinds of different monomers)
To refer to the polymer prepared by three kinds of different monomers).It also includes the polymer manufactured by polymerizeing more kinds of monomers.
" blend " means the polymer that two or more polymer is formed by mixing jointly by physics or chemical method.
One aspect of the present invention provides a kind of electrospinning nylon 46/PVA/ boric acid composite nano fibers, the composite Nano
Fiber includes nylon 46 salt, molecular adhesion agent and heat-resisting additive, wherein the molecular adhesion agent is PVA, the heat-resisting addition
Agent is boric acid；The mass ratio of the nylon 46 salt and the PVA are (0.4~6)：1；Preferably, the nylon 46 salt with it is described
The mass ratio of PVA is (0.6~4)：1.
Nylon 46
What it is in nylon 46 amide groups is 4 methylene on one side, and another side is 6 methylene, so that each given chain
Amide groups number in length is more than nylon66 fiber, and the structure height of chemical chain is symmetrical.The structural symmetry of nylon 46 so that
Nylon 46 has perfect crystal structure, and compared with other engineering plastics, non-reinforced nylon 46 has just shown very outstanding
Shock resistance.Even if in lower temperature, Izod notch impact strengths are still maintained at higher level.Nylon 46 it is perfect
Crystal structure and high-crystallinity impart its excellent rub resistance ability, the friction coefficient and polyformaldehyde (POM) of nylon 46 connect
Closely, abrasion resistance properties are better than POM, therefore nylon 46 is made to be widely used in high-temperature wearable wiping, anti-abrasive material.
PVA
Polyvinyl alcohol, organic compound, white plates, cotton-shaped or pulverulent solids are tasteless.It is dissolved in water (95 DEG C or more),
Insoluble in gasoline, kerosene, vegetable oil, benzene, toluene, dichloroethanes, carbon tetrachloride, acetone, ethyl acetate, methanol, ethylene glycol etc..
It is slightly soluble in dimethyl sulfoxide (DMSO).Polyvinyl alcohol is important industrial chemicals, for manufacturing Pioloform, polyvinyl acetal, resistance to gasoline pipeline and dimension
Nylon synthetic fibers, fabric-treating agent, emulsifier, paper coating, adhesive, glue etc..
Boric acid
Boric acid has satiny feel, odorless for white powder crystallization or the crystallization of three clinopinacoid flakey gloss.It is dissolved in
In water, alcohol, glycerine, ethers and essential oil, aqueous solution is weakly acidic.It is (optical glass, acid-resistant glass, resistance to be largely used to glass
Hot glass, insulating materials glass fibre) industry, heat-resisting, the transparent performance of glassware can be improved, improve mechanical strength,
Shortening dissolves the time.
In one embodiment, the mass ratio of the PVA and the boric acid is (1~6)：1.
In one embodiment, the mass ratio of the PVA and the boric acid is (1~5)：1；Preferably, the PVA with
The mass ratio of the boric acid is (1.5~4)：1.
In one embodiment, the weight average molecular weight of the PVA is 1.6 × 104~1 × 105g/mol；It is preferably described
The weight average molecular weight of PVA is 1.6 × 104~5 × 104g/mol。
After weight average molecular weight carries out polystyrene conversion based on gel permeation chromatography (referred to as " GPC ") measurement
Value.The determination condition of GPC uses the condition test of this field routine, tests to obtain for example, following modes can be used.
Column：Following columns are connected in series with and are used.
" TSKgelG5000 " (7.8mmI.D. × 30cm) × 1 piece
" TSKgelG4000 " (7.8mmI.D. × 30cm) × 1 piece
" TSKgelG3000 " (7.8mmI.D. × 30cm) × 1 piece
" TSKgelG2000 " (7.8mmI.D. × 30cm) × 1 piece
Detector：RI (differential refractometer)；Column temperature：40℃；Eluent：Tetrahydrofuran (THF)；Flow velocity：1.0mL/ point
Clock；Injection rate：100 μ L (tetrahydrofuran solution of sample solution concentration 4mg/mL)；Standard sample：Use following monodisperse polystyrenes
Alkene makes standard curve.
Another aspect of the present invention provides a kind of preparation method of electrospinning nylon 46/PVA/ boric acid composite nano fibers, packet
Include following steps：
(1) sample dissolves：Nylon 46 salt is dissolved in deionized water；
(2) raw material mixes：PVA, boric acid are added in step (1) solution in mass ratio, stirred, is uniformly mixed, obtains
To nylon 46 salt/PVA/ boric acid mixed solutions；
(3) electrostatic spinning：The step (2) nylon 46 salt/PVA/ boric acid mixed solutions are prepared into nylon by electrospinning
46 salt/PVA/ boric acid precursor；
(4) it is heat-treated：The step (3) nylon 46 salt/PVA/ boric acid mixed solutions are prepared into nylon 46 salt/PVA/ boron
Sour precursor is dried, and after heat treatment, obtains the nylon 46/PVA/ boric acid composite nano fibers.
Electrostatic spinning
Electrostatic spinning is a kind of special fiber fabrication process, and polymer solution or melt carry out injection spinning in highfield
Silk.Under electric field action, the drop at syringe needle can be become conical (i.e. " taylor cone ") from spherical shape, and be extended from conical tip
To fiber filaments.This mode can produce the polymer filaments of nanometer grade diameter.
In one embodiment, nylon 46 salt and the mass ratio of the deionized water described in the step (1) are
(0.3~0.5)：1；Preferably, the mass ratio of nylon 46 salt described in the step (1) and the deionized water be (0.3~
0.4)：1；It is highly preferred that nylon 46 salt described in the step (1) and the mass ratio of the deionized water are (0.35~0.4)：
1。
In one embodiment, in the step (2) nylon 46 salt/PVA/ boric acid mixed solutions total concentration be 10~
25%；Preferably, the total concentration of nylon 46 salt/PVA/ boric acid mixed solutions is 15~20% in the step (2).
In one embodiment, in the step (2) nylon 46 salt/PVA/ boric acid mixed solutions absolute viscosity 1.0-
3.6Pa/s；Preferably, in the step (2) nylon 46 salt/PVA/ boric acid mixed solutions absolute viscosity 1.5-3.0Pa/s.
In one embodiment, the electrostatic spinning temperature is 5~30 DEG C；Preferably, the electrostatic spinning temperature is
15~25 DEG C.
In one embodiment, the spinning voltage is 10~40KV；Preferably, the spinning voltage be 10~
30KV；It is highly preferred that the spinning voltage is 20~30KV.
In one embodiment, it is 10~40cm that the spinning, which receives distance i.e. solidification distance,；Preferably, the spinning
It is 15~30cm to receive distance；It is highly preferred that it is 18cm that the spinning, which receives distance,.
In one embodiment, drying temperature described in the step (4) be 80~100 DEG C, drying time be 1.0~
2.0h；Preferably, drying temperature described in the step (4) is 90 DEG C, drying time 1.5h.
In one embodiment, heat treatment temperature described in the step (4) is 180~300 DEG C, and heat treatment time is
0.5~2h；Preferably, heat treatment temperature described in the step (4) is 200~250 DEG C, and heat treatment time is 1~1.5h.
In one embodiment, a diameter of 10~400nm of the nylon 46/PVA/ boric acid composite nano fibers；It is excellent
Selection of land, a diameter of 50~300nm of the nylon 46/PVA/ boric acid composite nano fibers；It is highly preferred that the nylon 46/
A diameter of 200~240nm of PVA/ boric acid composite nano fibers.
In one embodiment, the electrospinning nylon 46/PVA/ boric acid composite nano fibers are applied to non-woven cloth collar
Domain.
It is raw material that the present invention, which uses nylon 46 salt, PVA and boric acid, and water is solvent, and composite Nano fibre is prepared in electrospinning
Dimension, on the one hand, high-temperature heat treatment (200 degree), nylon 46 salt is converted into nylon 46 (polyamide), while PVA is acted on by boric acid
Not oxidized decomposition under 200 degree, obtained nylon 46/PVA/ boric acid composite nano fibers have better tensile strength, toughness,
Modulus and moderate elongation；On the other hand, since the fibre diameter of nylon nano fiber is small, flexible, the high spy of intensity
Point is equally had better tensile strength using nylon 46 produced by the present invention/PVA/ boric acid nano-fiber for production of non-woven and broken
Split elongation, the good feature of filterability.
The present invention, as solvent, nylon 46/PVA/ boric acid is prepared using Electrospinning Method using water safe and environment-friendly, at low cost
Composite nano fiber overcomes since formic acid taste is big, is not suitable for large-scale electrospinning from formic acid solution and prepares nylon nano
The shortcomings that fiber.
The equipment used when heretofore described electrostatic spinning is the FM- of the rich friendly horse science and technology limited Company production in Beijing
Type B electrospinning equipment (- 5~50kV).200 DEG C or more of heat treatment SKGL-1200 high temperature in the heat treatment step
Tube type resistance furnace is handled.
The present invention is specifically described below by embodiment.It is necessarily pointed out that following embodiment is only used
In the invention will be further described, it should not be understood as limiting the scope of the invention, professional and technical personnel in the field
Some the nonessential modifications and adaptations made according to the content of aforementioned present invention, still fall within protection scope of the present invention.
In addition, if without other explanations, it is raw materials used to be all commercially available, it is purchased from traditional Chinese medicines chemical reagent.
Embodiment 1
The preparation method of electrospinning nylon 46/PVA/ boric acid composite nano fibers, includes the following steps：
(1) sample dissolves：Nylon 46 salt is dissolved in deionized water, the matter of the nylon 46 salt and the deionized water
Amount is than being 0.3：1；
(2) raw material mixes：PVA, boric acid are added in step (1) solution in mass ratio, stirred, is uniformly mixed, obtains
To nylon 46 salt/PVA/ boric acid mixed solutions, the mass ratio of the nylon 46 salt and the PVA are 0.4：1；The PVA and institute
The mass ratio for stating boric acid is 1：1；The weight average molecular weight of the PVA is 1.6 × 104g/mol；
(3) electrostatic spinning：The step (2) nylon 46 salt/PVA/ boric acid mixed solutions are prepared into nylon by electrospinning
46 salt/PVA/ boric acid precursor；The spinning voltage is 25KV；The electrostatic spinning temperature is 25 DEG C；The spinning receives distance
For 18cm；
(4) it is heat-treated：The step (3) nylon 46 salt/PVA/ boric acid mixed solutions are prepared into nylon 46 salt/PVA/ boron
Sour precursor is dried, and after heat treatment, obtains the nylon 46/PVA/ boric acid composite nano fibers；The drying temperature is 80
DEG C, drying time 2.0h；Heat treatment temperature is 200 DEG C, heat treatment time 1h.
Embodiment 2
The preparation method of electrospinning nylon 46/PVA/ boric acid composite nano fibers, includes the following steps：
(1) sample dissolves：Nylon 46 salt is dissolved in deionized water, the matter of the nylon 46 salt and the deionized water
Amount is than being 0.32：1；
(2) raw material mixes：PVA, boric acid are added in step (1) solution in mass ratio, stirred, is uniformly mixed, obtains
To nylon 46 salt/PVA/ boric acid mixed solutions, the mass ratio of the nylon 46 salt and the PVA are 0.6：1；The PVA and institute
The mass ratio for stating boric acid is 1.5：1；The weight average molecular weight of the PVA is 2 × 104g/mol；
(3) electrostatic spinning：The step (2) nylon 46 salt/PVA/ boric acid mixed solutions are prepared into nylon by electrospinning
46 salt/PVA/ boric acid precursor；The spinning voltage is 25KV；The electrostatic spinning temperature is 25 DEG C；The spinning receives distance
For 18cm；
(4) it is heat-treated：The step (3) nylon 46 salt/PVA/ boric acid mixed solutions are prepared into nylon 46 salt/PVA/ boron
Sour precursor is dried, and after heat treatment, obtains the nylon 46/PVA/ boric acid composite nano fibers；The drying temperature is 90
DEG C, drying time 1.6h；Heat treatment temperature is 200 DEG C, heat treatment time 1h.
Embodiment 3
The preparation method of electrospinning nylon 46/PVA/ boric acid composite nano fibers, includes the following steps：
(1) sample dissolves：Nylon 46 salt is dissolved in deionized water, the matter of the nylon 46 salt and the deionized water
Amount is than being 0.35：1；
(2) raw material mixes：PVA, boric acid are added in step (1) solution in mass ratio, stirred, is uniformly mixed, obtains
To nylon 46 salt/PVA/ boric acid mixed solutions, the mass ratio of the nylon 46 salt and the PVA are 1：1；The PVA with it is described
The mass ratio of boric acid is 2：1；The weight average molecular weight of the PVA is 3 × 104g/mol；
(3) electrostatic spinning：The step (2) nylon 46 salt/PVA/ boric acid mixed solutions are prepared into nylon by electrospinning
46 salt/PVA/ boric acid precursor；The spinning voltage is 25KV；The electrostatic spinning temperature is 25 DEG C；The spinning receives distance
For 18cm；
(4) it is heat-treated：The step (3) nylon 46 salt/PVA/ boric acid mixed solutions are prepared into nylon 46 salt/PVA/ boron
Sour precursor is dried, and after heat treatment, obtains the nylon 46/PVA/ boric acid composite nano fibers；The drying temperature is 100
DEG C, drying time 1.0h；Heat treatment temperature is 200 DEG C, heat treatment time 2h.
Embodiment 4
The preparation method of electrospinning nylon 46/PVA/ boric acid composite nano fibers, includes the following steps：
(1) sample dissolves：Nylon 46 salt is dissolved in deionized water, the matter of the nylon 46 salt and the deionized water
Amount is than being 0.37：1；
(2) raw material mixes：PVA, boric acid are added in step (1) solution in mass ratio, stirred, is uniformly mixed, obtains
To nylon 46 salt/PVA/ boric acid mixed solutions, the mass ratio of the nylon 46 salt and the PVA are 2：1；The PVA with it is described
The mass ratio of boric acid is 3：1；The weight average molecular weight of the PVA is 4 × 104g/mol；
(3) electrostatic spinning：The step (2) nylon 46 salt/PVA/ boric acid mixed solutions are prepared into nylon by electrospinning
46 salt/PVA/ boric acid precursor；The spinning voltage is 25KV；The electrostatic spinning temperature is 25 DEG C；The spinning receives distance
For 18cm；
(4) it is heat-treated：The step (3) nylon 46 salt/PVA/ boric acid mixed solutions are prepared into nylon 46 salt/PVA/ boron
Sour precursor is dried, and after heat treatment, obtains the nylon 46/PVA/ boric acid composite nano fibers；The drying temperature is 80
DEG C, drying time 2.0h；Heat treatment temperature is 200 DEG C, heat treatment time 2h.
Embodiment 5
The preparation method of electrospinning nylon 46/PVA/ boric acid composite nano fibers, includes the following steps：
(1) sample dissolves：Nylon 46 salt is dissolved in deionized water, the matter of the nylon 46 salt and the deionized water
Amount is than being 0.6：1；
(2) raw material mixes：PVA, boric acid are added in step (1) solution in mass ratio, stirred, is uniformly mixed, obtains
To nylon 46 salt/PVA/ boric acid mixed solutions, the mass ratio of the nylon 46 salt and the PVA are 4：1；The PVA with it is described
The mass ratio of boric acid is 4：1；The weight average molecular weight of the PVA is 5 × 104g/mol；
(3) electrostatic spinning：The step (2) nylon 46 salt/PVA/ boric acid mixed solutions are prepared into nylon by electrospinning
46 salt/PVA/ boric acid precursor；The spinning voltage is 25KV；The electrostatic spinning temperature is 25 DEG C；The spinning receives distance
For 18cm；
(4) it is heat-treated：The step (3) nylon 46 salt/PVA/ boric acid mixed solutions are prepared into nylon 46 salt/PVA/ boron
Sour precursor is dried, and after heat treatment, obtains the nylon 46/PVA/ boric acid composite nano fibers；The drying temperature is 80
DEG C, drying time 2.0h；Heat treatment temperature is 200 DEG C, heat treatment time 1h.
Embodiment 6
The preparation method of electrospinning nylon 46/PVA/ boric acid composite nano fibers, includes the following steps：
(1) sample dissolves：Nylon 46 salt is dissolved in deionized water, the matter of the nylon 46 salt and the deionized water
Amount is than being 0.37：1；
(2) raw material mixes：PVA, boric acid are added in step (1) solution in mass ratio, stirred, is uniformly mixed, obtains
To nylon 46 salt/PVA/ boric acid mixed solutions, the mass ratio of the nylon 46 salt and the PVA are 3.2：1；The PVA and institute
The mass ratio for stating boric acid is 2.4：1；The weight average molecular weight of the PVA is 2.8 × 104g/mol；
(3) electrostatic spinning：The step (2) nylon 46 salt/PVA/ boric acid mixed solutions are prepared into nylon by electrospinning
46 salt/PVA/ boric acid precursor；The spinning voltage is 25KV；The electrostatic spinning temperature is 25 DEG C；The spinning receives distance
For 18cm；
(4) it is heat-treated：The step (3) nylon 46 salt/PVA/ boric acid mixed solutions are prepared into nylon 46 salt/PVA/ boron
Sour precursor is dried, and after heat treatment, obtains the nylon 46/PVA/ boric acid composite nano fibers；The drying temperature is 90
DEG C, drying time 1.6h；Heat treatment temperature is 200 DEG C, heat treatment time 1.5h.
Comparative example 1
Commercially available nylon 46.It buys from Tianjin Heowns Biochemical Technology Co., Ltd., product specification：50g, purity 98%.
Comparative example 2
The preparation method of electrospinning nylon 46/PVA composite nano fibers, includes the following steps：
(1) sample dissolves：Nylon 46 salt is dissolved in deionized water, the matter of the nylon 46 salt and the deionized water
Amount is than being 0.37：1；
(2) raw material mixes：PVA is added in the step (1) solution in mass ratio, is stirred, is uniformly mixed, obtains nylon
The mass ratio of 46 salt/PVA mixed solutions, the nylon 46 salt and the PVA are 3.2：1；The weight average molecular weight of the PVA is
2.8×104g/mol；
(3) electrostatic spinning：By electrospinning by the step (2) nylon 46 salt/PVA mixed solutions be prepared into nylon 46 salt/
PVA precursor；The spinning voltage is 25KV；The electrostatic spinning temperature is 25 DEG C；It is 18cm that the spinning, which receives distance,；
(4) it is heat-treated：The step (3) nylon 46 salt/PVA mixed solutions are prepared into nylon 46 salt/PVA precursor to carry out
It is dry, after heat treatment, obtain the nylon 46/PVA composite nano fibers；The drying temperature is 90 DEG C, and drying time is
1.6h；Heat treatment temperature is 200 DEG C, heat treatment time 1.5h.
Comparative example 3
The preparation method of electrospinning nylon66 fiber/PVA/ boric acid composite nano fibers, includes the following steps：
(1) sample dissolves：Nylon salt is dissolved in deionized water, the matter of the nylon salt and the deionized water
Amount is than being 0.37：1；
(2) raw material mixes：PVA, boric acid are added in step (1) solution in mass ratio, stirred, is uniformly mixed, obtains
To nylon salt/PVA/ boric acid mixed solutions, the mass ratio of the nylon salt and the PVA are 3.2：1；The PVA and institute
The mass ratio for stating boric acid is 2.4：1；The weight average molecular weight of the PVA is 2.8 × 104g/mol；
(3) electrostatic spinning：The step (2) nylon salt/PVA/ boric acid mixed solutions are prepared into nylon by electrospinning
66 salt/PVA/ boric acid precursor；The spinning voltage is 25KV；The electrostatic spinning temperature is 25 DEG C；The spinning receives distance
For 18cm；
(4) it is heat-treated：The step (3) nylon salt/PVA/ boric acid mixed solutions are prepared into nylon salt/PVA/ boron
Sour precursor is dried, and after heat treatment, obtains the nylon66 fiber/PVA/ boric acid composite nano fibers；The drying temperature is 90
DEG C, drying time 1.6h；Heat treatment temperature is 200 DEG C, heat treatment time 1.5h.
Non-woven cloth
The composite nano fiber being prepared using embodiment 1-6 and comparative example 1~3 is made non-as raw material, using fusion method
Woven cloths.Specifically comprise the steps of：
Melt simultaneously force feed melt to polymer chips using screw extruder；Polymer melt enter spinneret die it
It is preceding to be filtered through multilayer detailed catalogue metallic sieve；Gear wheel metering pump carries out melt-stoichiometry, and polymer melt is sent after accurate metering to molten
Jet mould head；After melt is transported to die head, it is evenly dispersed to each spinneret orifice by runner, and sprayed through spinneret orifice；From mould
While puffing swell occurs for the melt stream that head spinneret orifice squeezes out, by the drawing-off of both sides high velocity, hot air stream, it is in viscosity flow
The melt stream of state is drawn and attenuated rapidly, meanwhile, the air at room temperature of both sides mixes drawing-off stream of hot air, and melt stream is made to cool and solidify
Forming forms superfine fibre；Superfine fibre through drawing-off and cooling and solidifying blows to solidifying lace curtaining or rolling under the action of attenuating blast
Cylinder, fiber are collected on solidifying lace curtaining or roller, and nano-fiber for production of non-woven is formed.
Performance test：
1. fibre diameter measures
Pattern and fibre diameter carry out observation survey using scanning electron microscope (VEGA3LMU, Tescan companies of Czech)
It is fixed；
2. the measurement of the tensile strength of fibre single thread (bioassay standard uses GB 9997-88)
It is measured, the result of each sample using JQ03new type Miniature tensions instrument (upper marine morning Digital Equipment Co., Ltd)
It is obtained by the average value of 10 this group of samples；
3. fibre single thread is broken the measurement of percentage of elongation (bioassay standard uses GB 9997-88)
It is measured with the miniature control electronic universal testers of CMT8102 (Shenzhen SANS material tests Co., Ltd)；
4. the measurement of Young's modulus
It is measured using YMC-1 measure apparatus of youngs modulus (Changchun Great Wall instruments used for education Co., Ltd)；
5. electro spinning nano fiber non-woven cloth is broken the measurement of percentage of elongation
It is measured with the miniature control electronic universal testers of CMT8102 (Shenzhen SANS material tests Co., Ltd)；
6. the measurement of electro spinning nano fiber non-woven cloth tensile strength
It is measured with the miniature control electronic universal testers of CMT8102 (Shenzhen SANS material tests Co., Ltd)；
7. the measurement of electro spinning nano fiber non-woven cloth Young's modulus
It is measured using YMC-1 measure apparatus of youngs modulus (Changchun Great Wall instruments used for education Co., Ltd).
1 the performance test results of table
From above-mentioned data result can be seen that by with nylon 46, electrospinning nylon 46/PVA composite nano fibers and electrospinning
Nylon66 fiber/PVA/ boric acid composite nano fibers are compared, electrospinning nylon 46/PVA/ boric acid composite nano fiber of the present invention and its
Non-woven cloth all has good tensile strength and modulus, excellent chemical resistance and heat resistance, high temperature filtration and harsh chemical
Environment filtration field has very big potential application.
Example above-mentioned is merely illustrative, some features of the feature for explaining the disclosure, those skilled in the art
Present disclosure can be used for reference, technological parameter realization is suitably modified.In particular, it should be pointed out that all similar substitutions and modifications pair
It is it will be apparent that they are considered as being included in the present invention for those skilled in the art.The method of the present invention and application are
Be described through passing through preferred embodiment, related personnel obviously can not depart from the content of present invention, in spirit and scope to this
Methods and applications described in text are modified or suitably change and combine, to realize and apply the technology of the present invention.
Claims (9)
1. a kind of electrospinning nylon 46/PVA/ boric acid composite nano fibers, which is characterized in that the composite nano fiber includes nylon
46 salt, molecular adhesion agent and heat-resisting additive, wherein the molecular adhesion agent is PVA, and the heat-resisting additive is boric acid；Institute
The mass ratio for stating nylon 46 salt and the PVA is (0.4~6)：1；
The preparation method of the electrospinning nylon 46/PVA/ boric acid composite nano fibers, includes the following steps：
(1) sample dissolves：Nylon 46 salt is dissolved in deionized water；
(2) raw material mixes：PVA, boric acid are added in step (1) solution in mass ratio, stirred, is uniformly mixed, obtains Buddhist nun
Imperial 46 salt/PVA/ boric acid mixed solutions；
(3) electrostatic spinning：By electrospinning by the step (2) nylon 46 salt/PVA/ boric acid mixed solutions be prepared into nylon 46 salt/
PVA/ boric acid precursor；
(4) it is heat-treated：It is former that the step (3) nylon 46 salt/PVA/ boric acid mixed solutions are prepared into nylon 46 salt/PVA/ boric acid
Silk is dried, and after heat treatment, obtains the nylon 46/PVA/ boric acid composite nano fibers.
2. electrospinning nylon 46/PVA/ boric acid composite nano fibers according to claim 1, which is characterized in that the PVA and institute
The mass ratio for stating boric acid is (1~6)：1.
3. electrospinning nylon 46/PVA/ boric acid composite nano fibers according to claim 2, which is characterized in that the PVA and institute
The mass ratio for stating boric acid is (1~5)：1.
4. electrospinning nylon 46/PVA/ boric acid composite nano fibers according to claim 1, which is characterized in that the weight of the PVA
Average molecular weight is 1.6 × 104~1 × 105g/mol。
5. the preparation method of electrospinning nylon 46/PVA/ boric acid composite nano fibers according to claim 1, which is characterized in that
Nylon 46 salt described in the step (1) and the mass ratio of the deionized water are (0.3~0.5)：1.
6. the preparation method of electrospinning nylon 46/PVA/ boric acid composite nano fibers according to claim 1, which is characterized in that
Drying temperature described in the step (4) is 80~100 DEG C, and drying time is 1.0~2.0h.
7. the preparation method of electrospinning nylon 46/PVA/ boric acid composite nano fibers according to claim 1, which is characterized in that
Heat treatment temperature described in the step (4) is 180~300 DEG C, and heat treatment time is 0.5~2h.
8. the preparation method of electrospinning nylon 46/PVA/ boric acid composite nano fibers according to claim 1, which is characterized in that
A diameter of 10~400nm of the nylon 46/PVA/ boric acid composite nano fibers.
9. electrospinning nylon 46/PVA/ boric acid composite nano fibers according to claim 1, which is characterized in that the electrospinning Buddhist nun
Imperial 46/PVA/ boric acid composite nano fiber is applied to Nonwovens Field.
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| CN101502759A (en) * | 2009-02-05 | 2009-08-12 | 东华大学 | Method for preparing nylon 6/chitosan superfine nano fiber film by electrostatic blended spinning process |
| CN104805535A (en) * | 2015-04-14 | 2015-07-29 | 华南理工大学 | Preparation method of porous carbon nanofiber |
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| CN101502759A (en) * | 2009-02-05 | 2009-08-12 | 东华大学 | Method for preparing nylon 6/chitosan superfine nano fiber film by electrostatic blended spinning process |
| CN104805535A (en) * | 2015-04-14 | 2015-07-29 | 华南理工大学 | Preparation method of porous carbon nanofiber |
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