CN106223019A - A kind of preparation method of cross-linking polyvinyl alcohol nano fibrous membrane - Google Patents

A kind of preparation method of cross-linking polyvinyl alcohol nano fibrous membrane Download PDF

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Publication number
CN106223019A
CN106223019A CN201610699394.3A CN201610699394A CN106223019A CN 106223019 A CN106223019 A CN 106223019A CN 201610699394 A CN201610699394 A CN 201610699394A CN 106223019 A CN106223019 A CN 106223019A
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CN
China
Prior art keywords
pva
fibrous membrane
nano fibrous
exsiccator
dividing plate
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CN201610699394.3A
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Chinese (zh)
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王利萍
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Individual
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Individual
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Priority to CN201610699394.3A priority Critical patent/CN106223019A/en
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/12Aldehydes; Ketones
    • D06M13/123Polyaldehydes; Polyketones
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0015Electro-spinning characterised by the initial state of the material
    • D01D5/003Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0069Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4282Addition polymers
    • D04H1/4309Polyvinyl alcohol
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/07Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/11Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/18Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/24Polymers or copolymers of alkenylalcohols or esters thereof; Polymers or copolymers of alkenylethers, acetals or ketones

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Artificial Filaments (AREA)

Abstract

A kind of preparation method of cross-linking polyvinyl alcohol nano fibrous membrane, first prepare PVA nano fibrous membrane, prepare glutaraldehyde cross-linking PVA nano fibrous membrane, measure glutaraldehyde (GA) that 10mL mass fraction is 20% and 10mL mass fraction is the hydrochloric acid of 18%, pour in 2 identical culture dishs respectively, it is put into together exsiccator dividing plate lower end, variable color silica gel is put in exsiccator dividing plate upper end, Glass rod is put into exsiccator dividing plate upper end, PVA fibrous membrane is fixed on Glass rod, in the environment of room temperature is closed, carry out the gas phase crosslinking Treatment of 5.5h respectively.The invention has the beneficial effects as follows: synthesis technique is simple, reaction condition is gentle, and production cost is relatively low, favorable repeatability.

Description

A kind of preparation method of cross-linking polyvinyl alcohol nano fibrous membrane
Technical field
The present invention relates to material synthesis method, the preparation method of a kind of cross-linking polyvinyl alcohol nano fibrous membrane.
Background technology
Electrostatic spinning is simple by manufacturing device, and spinning is with low cost, it is easy to operation, the advantages such as technique is easily controllable, Through becoming the currently the only method that can prepare polymer nanofiber directly, continuously, also it is to prepare nanofiber the most simply to have The method of effect, and play great function in fields such as food, cosmetics, biomedicine, the energy, filtering materials.
Polyvinyl alcohol (PVA) is a kind of water soluble polyhydroxy polymer, has good chemical stability and bio-compatible Property and degradability, avirulence, have preferable hydrophilic, have extensively at aspects such as medical material, cosmetics, food engineerings water General application.Using biocompatible PVA is macromolecule, is solvent with water, it is also possible to avoid making of toxic organic solvent With.
PVA can be made nano fibrous membrane by electrostatic spinning technique, possess the stronger absorption affinity of film and relatively The characteristics such as good filterability, cohesive and heat insulating ability.But there is substantial amounts of hydrophilic group on the main chain of PVA, cause PVA Nano fibrous membrane water absorption is strong, is prone to dissolve, has a strong impact on the processing of PVA nano fibrous membrane and make in moist environment Use performance.
Summary of the invention
The technical problem to be solved is to provide the preparation method of a kind of cross-linking polyvinyl alcohol nano fibrous membrane, A kind of new synthetic method is provided.
The synthetic method that the present invention uses, comprises the steps:
A, preparation PVA nano fibrous membrane, be dissolved in PVA in the mixed solution of ultra-pure water and formic acid volume ratio 3:1, be placed in 80 DEG C constant temperature oscillator in dissolve 12h, prepared mass fraction is the PVA solution of 12.5%, the PVA spinning that will have configured Liquid is poured in the 5mL glass syringe being furnished with 9# rustless steel syringe needle, uses the syringe needle scabbled as nozzle needle, and internal diameter is 0.7mm, Nozzle needle connects the positive pole of high voltage power supply, and aluminium foil fiber receives plate and connects its negative pole, and spray volume is set by syringe pump control, injection electric Being set to 12kV, the distance between nozzle needle and aluminium foil is 15cm, spinning speed 0.6mL/h, and ambient temperature (20 ± 5) DEG C is the wettest Degree 30% ± 5%;
B, prepare glutaraldehyde cross-linking PVA nano fibrous membrane, measure glutaraldehyde (GA) that 10mL mass fraction is 20% and 10mL mass fraction is the hydrochloric acid of 18%, pours into respectively in 2 identical culture dishs, it is put into together under exsiccator dividing plate End, puts variable color silica gel in exsiccator dividing plate upper end, Glass rod is put into exsiccator dividing plate upper end, PVA fibrous membrane is fixed on On Glass rod, in the environment of room temperature is closed, carry out the gas phase crosslinking Treatment of 5.5h respectively.
The invention has the beneficial effects as follows: synthesis technique is simple, reaction condition is gentle, and production cost is relatively low, favorable repeatability.
Detailed description of the invention
Further illustrating present disclosure below in conjunction with example, as known by the technical knowledge, the present invention also can pass through other The scheme without departing from the technology of the present invention feature describe, the most all within the scope of the present invention or equivalent the scope of the invention in Change and be all included in the invention.
Embodiment 1:
A, preparation PVA nano fibrous membrane, be dissolved in PVA in the mixed solution of ultra-pure water and formic acid volume ratio 3:1, be placed in 80 DEG C constant temperature oscillator in dissolve 12h, prepared mass fraction is the PVA solution of 12.5%, the PVA spinning that will have configured Liquid is poured in the 5mL glass syringe being furnished with 9# rustless steel syringe needle, uses the syringe needle scabbled as nozzle needle, and internal diameter is 0.7mm, Nozzle needle connects the positive pole of high voltage power supply, and aluminium foil fiber receives plate and connects its negative pole, and spray volume is set by syringe pump control, injection electric Being set to 12kV, the distance between nozzle needle and aluminium foil is 15cm, spinning speed 0.6mL/h, ambient temperature (20+5) DEG C, relative humidity 30%+5%;
B, prepare glutaraldehyde cross-linking PVA nano fibrous membrane, measure glutaraldehyde (GA) that 10mL mass fraction is 20% and 10mL mass fraction is the hydrochloric acid of 18%, pours into respectively in 2 identical culture dishs, it is put into together under exsiccator dividing plate End, puts variable color silica gel in exsiccator dividing plate upper end, Glass rod is put into exsiccator dividing plate upper end, PVA fibrous membrane is fixed on On Glass rod, in the environment of room temperature is closed, carry out the gas phase crosslinking Treatment of 5.5h respectively.
Embodiment 2:
A, preparation PVA nano fibrous membrane, be dissolved in PVA in the mixed solution of ultra-pure water and formic acid volume ratio 3:1, be placed in 80 DEG C constant temperature oscillator in dissolve 12h, prepared mass fraction is the PVA solution of 12.5%, the PVA spinning that will have configured Liquid is poured in the 5mL glass syringe being furnished with 9# rustless steel syringe needle, uses the syringe needle scabbled as nozzle needle, and internal diameter is 0.7mm, Nozzle needle connects the positive pole of high voltage power supply, and aluminium foil fiber receives plate and connects its negative pole, and spray volume is set by syringe pump control, injection electric Being set to 12kV, the distance between nozzle needle and aluminium foil is 15cm, spinning speed 0.6mL/h, ambient temperature (20-5) DEG C, relative humidity 30%-5%;
B, prepare glutaraldehyde cross-linking PVA nano fibrous membrane, measure glutaraldehyde (GA) that 10mL mass fraction is 20% and 10mL mass fraction is the hydrochloric acid of 18%, pours into respectively in 2 identical culture dishs, it is put into together under exsiccator dividing plate End, puts variable color silica gel in exsiccator dividing plate upper end, Glass rod is put into exsiccator dividing plate upper end, PVA fibrous membrane is fixed on On Glass rod, in the environment of room temperature is closed, carry out the gas phase crosslinking Treatment of 5.5h respectively.
By experiment, when PVA mass fraction is 12.5%, best by SEM photograph fiber morphology.
By experiment, when crosslinking time is 5.5h, the water absorbent rate of fibrous membrane reaches maximum, for 905g/g.

Claims (1)

1. a preparation method for cross-linking polyvinyl alcohol nano fibrous membrane, comprises the steps:
A, preparation PVA nano fibrous membrane, be dissolved in PVA in the mixed solution of ultra-pure water and formic acid volume ratio 3:1, be placed in 80 DEG C constant temperature oscillator in dissolve 12h, prepared mass fraction is the PVA solution of 12.5%, the PVA spinning that will have configured Liquid is poured in the 5mL glass syringe being furnished with 9# rustless steel syringe needle, uses the syringe needle scabbled as nozzle needle, and internal diameter is 0.7mm, Nozzle needle connects the positive pole of high voltage power supply, and aluminium foil fiber receives plate and connects its negative pole, and spray volume is set by syringe pump control, injection electric Being set to 12kV, the distance between nozzle needle and aluminium foil is 15cm, spinning speed 0.6mL/h, and ambient temperature (20 ± 5) DEG C is the wettest Degree 30% ± 5%;
B, prepare glutaraldehyde cross-linking PVA nano fibrous membrane, measure glutaraldehyde (GA) that 10mL mass fraction is 20% and 10mL mass fraction is the hydrochloric acid of 18%, pours into respectively in 2 identical culture dishs, it is put into together under exsiccator dividing plate End, puts variable color silica gel in exsiccator dividing plate upper end, Glass rod is put into exsiccator dividing plate upper end, PVA fibrous membrane is fixed on On Glass rod, in the environment of room temperature is closed, carry out the gas phase crosslinking Treatment of 5.5h respectively.
CN201610699394.3A 2016-08-22 2016-08-22 A kind of preparation method of cross-linking polyvinyl alcohol nano fibrous membrane Pending CN106223019A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108654394A (en) * 2018-05-29 2018-10-16 南京林业大学 A kind of nanofiber cation-exchange membrane and the preparation method and application thereof
CN111876405A (en) * 2020-08-10 2020-11-03 山东华熙海御生物医药有限公司 Method for immobilizing enzyme on nanofiber

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1600855A (en) * 2004-08-06 2005-03-30 天津大学 Nano superfine fiber membrane of polyvinyl alcohol with immovable cellulase

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1600855A (en) * 2004-08-06 2005-03-30 天津大学 Nano superfine fiber membrane of polyvinyl alcohol with immovable cellulase

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
朱广千 等: "交联聚乙烯醇纳米纤维膜的制备与性能研究", 《化工新型材料》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108654394A (en) * 2018-05-29 2018-10-16 南京林业大学 A kind of nanofiber cation-exchange membrane and the preparation method and application thereof
CN108654394B (en) * 2018-05-29 2020-08-25 南京林业大学 Nanofiber cation exchange membrane and preparation method and application thereof
CN111876405A (en) * 2020-08-10 2020-11-03 山东华熙海御生物医药有限公司 Method for immobilizing enzyme on nanofiber
CN111876405B (en) * 2020-08-10 2022-07-15 山东华熙海御生物医药有限公司 Method for immobilizing enzyme on nano fiber

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Application publication date: 20161214