CN108728929A - A kind of nano-fiber material and preparation method thereof of filtering heavy metal ion - Google Patents

A kind of nano-fiber material and preparation method thereof of filtering heavy metal ion Download PDF

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Publication number
CN108728929A
CN108728929A CN201810520370.6A CN201810520370A CN108728929A CN 108728929 A CN108728929 A CN 108728929A CN 201810520370 A CN201810520370 A CN 201810520370A CN 108728929 A CN108728929 A CN 108728929A
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heavy metal
metal ion
nano
fiber material
pan
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CN108728929B (en
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兰清泉
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Zeta Nanotechnology (suzhou) Co Ltd
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Zeta Nanotechnology (suzhou) Co Ltd
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/02—Loose filtering material, e.g. loose fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28023—Fibres or filaments
    • 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
    • D01F8/08—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyacrylonitrile as constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/02—Types of fibres, filaments or particles, self-supporting or supported materials
    • B01D2239/0208—Single-component fibres

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

This application involves a kind of nano-fiber materials and preparation method thereof of filtering heavy metal ion.The application is by using graphene oxide, polyacrylonitrile (PAN) and polymetylmethacrylate as raw material; the nanofiber of high-specific surface area, fibre diameter, high stability has been prepared using solution spray spinning technique; there is excellent filtering suction-operated to the heavy metal ion in industrial wastewater; the preparation method production efficiency is high, production cost is low, simple for process and even in fiber diameter distribution; it is high to the filtering adsorption efficiency of heavy metal ion; removal is thorough, is suitable for scale industrial production.

Description

A kind of nano-fiber material and preparation method thereof of filtering heavy metal ion
Technical field
This application involves a kind of nano-fiber materials and preparation method thereof of filtering heavy metal ion.
Background technology
With the fast development of process of industrialization, the discharge capacity of industrial wastewater is growing day by day, containing a large amount of in industrial wastewater Heavy metal ion, heavy metal is difficult to degrade in the natural environment, difficult, its direct emission is entered in natural water body, can cause to give birth to State is destroyed or even some heavy metal ion have high toxicity, by being incremented by step by step for food chain, is gradually tired out in animal and plant body Product, increasing concen-trations, and finally cause serious injury to health with the intake of the mankind, such as protein in heavy metal and human body Situations such as reaction makes its inactivation, leads to heavy metal poisoning.Therefore, when industrial wastewater discharge, heavy metal ion therein is carried out It discharges after filtration treatment, is determined to win with reducing its subsequent contamination again.Conventional waste water processing mode has chemical method, ion exchange resin to hand over Change method, electrolysis, active carbon adsorption, hyperfiltration, electroosmose process, bioanalysis, evaporation concentration method etc., but its treatment effeciency It is low, production cost is high, and heavy metals removal is not thorough, therefore, how to provide a kind of mode of efficient removal metal pollutant at For urgent need to solve the problem instantly.
Graphene oxide GO is a kind of derivative of graphene, is by graphite oxide is peeling-off and is formed graphene Monolithic, have special single electron layer structure, and layer in combined with strong covalent bond, possess in graphene oxide structure hydroxyl, A large amount of oxygen-containing groups such as carboxyl, carbonyl and epoxy group, interlayer are connected with weak hydrogen bond by various oxygen-containing functional groups, are ultrasonically treated Under easily peeling-off dispersion, form uniform single-layer graphene oxide solution, the active function groups on surface are conducive to oxidation stone The further application of black alkene, therefore it is different in nature with graphene, graphene oxide GO belongs to a kind of hydrophily object Matter, and have the characteristics that specific surface area height, strong adsorption, use it for filtering, absorption industry using the active group on its surface Heavy metal ion in waste water has the advantages such as treatment effeciency is high, and removal is thorough.And graphene oxide itself is powder presence, it will It is melted or is dissolved to form spinning solution and carry out spinning moulding with polymer, is common molding side as fibrous material Method.
It is a kind of novel method for preparing micro nanometer fiber that solution, which sprays spinning technique, compared to traditional method of electrostatic spinning, It is not necessarily to electric field environment, does not need high-tension apparatus or any conductive collector, equipment is simpler, can be with higher injection speed Carry out spinning, easily operated, of low cost, spinning efficiency higher.The range of choice of polymer is more wide in range, is not limited only to have The polymer of high dielectric constant, and the solvent used is easy to volatilization and nontoxicity, it is more environmentally protective.Solution sprays spinning technique Polymer solution is handled by dissolving a polymer in volatile solvent, and using swiftly flowing gas-pressurized, it is molten to promote The volatilization of agent and the deposition refinement of fiber, to which fiber is deposited on substrate or carrier surface.It is prepared micro-nano Fiber has wider commercial value, is such as applied to enhancing by polymer object, therapeutic treatment, the filtering of PM2.5, electrical and optical device Part etc..
Invention content
For solve the problems, such as it is above-mentioned such as, the following technical solutions are proposed by concentrating on studies by spy.
A kind of nano-fiber material of filtering heavy metal ion is by graphene oxide, polyacrylonitrile (PAN) and poly- methyl Methyl acrylate PMMA is raw material, and spraying spinning technique by solution is prepared, wherein a concentration of 5~8wt% of graphene oxide, By weight, PAN：PMMA=1~10：10~1, fibre diameter is 30~500nm, and pulp freeness is 150~185m2/g。
Preferably, a concentration of 5~8wt% of graphene oxide, by weight, polyacrylonitrile (PAN)：Poly-methyl methacrylate Ester PMMA=2~8：8~2.
Preferably, the fibre diameter is 50~400nm, and pulp freeness is 160~185m2/g。
A kind of preparation method of the nano-fiber material of filtering heavy metal ion comprising following steps：
（1）PVP by weight：PMMA=1~10：10~1 ratio weighs polyacrylonitrile (PAN) and polymethyl methacrylate PMMA, and being dried in vacuo, PAN and PMMA are added in organic solvent, in 45 DEG C of ultrasonic agitations to being uniformly mixed, then are added Enter the graphene oxide of 5~8wt%, ultrasonic agitation obtains uniform dispersion, as polymer solution；The organic solvent is two Methyl sulfoxide, ethyl acetate, acetone, N, any one of N- dimethylformamides；
（2）By step（1）It configures obtained polymer solution through metering pump measure and enter spinning head, with polymer spun Silk solution squeezes out from spinneret orifice and is formed thread, while being blown thread progress high-speed flow using injection apparatus and penetrating and stretch, and obtains To the PAN/PMMA nanofibers being deposited on substrate, wherein stream pressure 50-80psi；
（3）To step（2）The nanofiber that is prepared carries out high-temperature thermal stability processing to get to filtering heavy metal ion Nano-fiber material.
Preferably, a concentration of 5~8wt% of graphene oxide, by weight, polyacrylonitrile (PAN)：Poly-methyl methacrylate Ester PMMA=2~8：8~2.
Preferably, step（1）Middle stream pressure is 70psi.
Preferably, a diameter of 50~400nm of the nano-fiber material for the filtering heavy metal ion being prepared, fiber Specific surface area is 160~185m2/g。
Advantageous effect
The advantageous effect that technical solution provided by the invention is brought is：Graphene oxide has larger specific surface area, higher Adsorption efficiency, and surface of graphene oxide contains abundant functional group, has excellent absorption property, the application to heavy metal By regarding graphene oxide, polyacrylonitrile (PAN) and polymetylmethacrylate as raw material, spinning technique system is sprayed using solution It is standby to have obtained the nanofiber of high-specific surface area, fibre diameter and high stability, and the concentration on fiber of polymer solution is straight Diameter is affected, and increases the concentration of polymer solution, and fibre diameter becomes larger, on the contrary, reducing the concentration of polymer solution, fiber is straight Diameter becomes smaller.This is because it is physical form to carry out the former driving force of spinning formation using solution spray spinning technique, and it polymerize species What type and concentration were to determine, the rheological behaviour and surface tension of solution directly affect the form and diameter of fiber.
By the preparation method production efficiency is high, production cost is low, simple for process and even in fiber diameter distribution, to a huge sum of money The filtering adsorption efficiency for belonging to ion is high, and removal is thorough, is suitable for scale industrial production.
Specific implementation mode
Embodiment 1
A kind of preparation method of the nano-fiber material of filtering heavy metal ion comprising following steps：
（1）PAN by weight：PMMA=5：8 ratio weighs polyacrylonitrile (PAN) and polymetylmethacrylate, and carries out Vacuum drying, PAN and PMMA are added in dimethyl sulfoxide (DMSO), in 45 DEG C of ultrasonic agitations to being uniformly mixed, add 5wt%'s Graphene oxide, ultrasonic agitation obtain uniform dispersion, as polymer solution；The concentration of PAN and PMMA be respectively 5wt% and 8wt%。
（2）By step（1）It configures obtained polymer solution through metering pump measure and enter spinning head, with polymerization Object spinning solution squeezes out from spinneret orifice and is formed thread, while being blown thread progress high-speed flow using injection apparatus and penetrating and draw It stretches, obtains being deposited on the PAN/PMMA nanofibers on substrate, wherein stream pressure 50psi；
（3）To step（2）The nanofiber that is prepared carries out high-temperature thermal stability processing to get to filtering heavy metal ion Nano-fiber material.Its fibre diameter is 240nm, pulp freeness 155m2/g。
Embodiment 2
A kind of preparation method of the nano-fiber material of filtering heavy metal ion comprising following steps：
（1）PAN by weight：PMMA=2：5 ratio weighs polyacrylonitrile (PAN) and polymetylmethacrylate, and carries out Vacuum drying, PAN and PMMA are added in dimethyl sulfoxide (DMSO), in 45 DEG C of ultrasonic agitations to being uniformly mixed, add 6wt%'s Graphene oxide, ultrasonic agitation obtain uniform dispersion, as polymer solution；The concentration of PAN and PMMA be respectively 2wt% and 5wt%。
（2）By step（1）It configures obtained polymer solution through metering pump measure and enter spinning head, with polymerization Object spinning solution squeezes out from spinneret orifice and is formed thread, while being blown thread progress high-speed flow using injection apparatus and penetrating and draw It stretches, obtains being deposited on the PAN/PMMA nanofibers on substrate, wherein stream pressure 50psi；
（3）To step（2）The nanofiber that is prepared carries out high-temperature thermal stability processing to get to filtering heavy metal ion Nano-fiber material.Its fibre diameter is 120nm, pulp freeness 150m2/g。
Embodiment 3
A kind of preparation method of the nano-fiber material of filtering heavy metal ion comprising following steps：
（1）PAN by weight：PMMA=8：6 ratio weighs polyacrylonitrile (PAN) and polymetylmethacrylate, and carries out Vacuum drying, PAN and PMMA are added in dimethyl sulfoxide (DMSO), in 45 DEG C of ultrasonic agitations to being uniformly mixed, add 7wt%'s Graphene oxide, ultrasonic agitation obtain uniform dispersion, as polymer solution；The concentration of PAN and PMMA be respectively 8wt% and 6wt%。
（2）By step（1）It configures obtained polymer solution through metering pump measure and enter spinning head, with polymerization Object spinning solution squeezes out from spinneret orifice and is formed thread, while being blown thread progress high-speed flow using injection apparatus and penetrating and draw It stretches, obtains being deposited on the PAN/PMMA nanofibers on substrate, wherein stream pressure 50psi；
（3）To step（2）The nanofiber that is prepared carries out high-temperature thermal stability processing to get to filtering heavy metal ion Nano-fiber material.Its fibre diameter is 300nm, pulp freeness 170m2/g。
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to be said using the present invention Equivalent structure or equivalent flow shift made by bright book content is applied directly or indirectly in other relevant technical fields, Similarly it is included within the scope of the present invention.

Claims (7)

1. a kind of filtering heavy metal ion nano-fiber material prepared using solution spray spinning technique, it is characterised in that the Nanowire It is raw material that dimension material, which is by graphene oxide, polyacrylonitrile (PAN) and polymetylmethacrylate, sprays spinning technique by solution It is prepared, wherein a concentration of 5~8wt% of graphene oxide, by weight, PAN：PMMA=1~10：10~1, fiber is straight Diameter is 30~500nm, and pulp freeness is 150~185m2/g。
2. a kind of nano-fiber material of filtering heavy metal ion according to claim 1, which is characterized in that graphite oxide A concentration of 5~8wt% of alkene, by weight, polyacrylonitrile (PAN)：Polymetylmethacrylate=2~8：8~2.
3. a kind of nano-fiber material of filtering heavy metal ion according to claim 1-2, which is characterized in that the fibre A diameter of 50~400nm is tieed up, pulp freeness is 160~185m2/g。
4. a kind of preparation method of filtering heavy metal ion nano-fiber material comprising following steps：
（1）PVP by weight：PMMA=1~10：10~1 ratio weighs polyacrylonitrile (PAN) and polymethyl methacrylate PMMA, and being dried in vacuo, PAN and PMMA are added in organic solvent, in 45 DEG C of ultrasonic agitations to being uniformly mixed, then are added Enter the graphene oxide of 5~8wt%, ultrasonic agitation obtains uniform dispersion, as polymer solution；The organic solvent is two Methyl sulfoxide, ethyl acetate, acetone, N, any one of N- dimethylformamides；
（2）By step（1）It configures obtained polymer solution through metering pump measure and enter spinning head, with polymer spun Silk solution squeezes out from spinneret orifice and is formed thread, while being blown thread progress high-speed flow using injection apparatus and penetrating and stretch, and obtains To the PAN/PMMA nanofibers being deposited on substrate, wherein stream pressure 50-80psi；
（3）To step（2）The nanofiber that is prepared carries out high-temperature thermal stability processing to get to filtering heavy metal ion Nano-fiber material.
5. a kind of preparation method of the nano-fiber material of filtering heavy metal ion according to claim 4, feature exist In, a concentration of 5~8wt% of graphene oxide, by weight, polyacrylonitrile (PAN)：Polymetylmethacrylate=2~8：8 ~2.
6. a kind of preparation method of the nano-fiber material of filtering heavy metal ion according to claim 4, feature exist In step（1）Middle stream pressure is 70psi.
7. a kind of preparation method of the nano-fiber material of filtering heavy metal ion according to claim 4, feature exist In, a diameter of 50~400nm of nano-fiber material for the filtering heavy metal ion being prepared, pulp freeness 160 ~185m2/g。
CN201810520370.6A 2018-05-28 2018-05-28 Nanofiber material for filtering heavy metal ions and preparation method thereof Active CN108728929B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110983478A (en) * 2019-11-28 2020-04-10 洪泽联合化纤有限公司 Preparation method of single-component fiber
CN112090169A (en) * 2020-08-12 2020-12-18 柳州紫荆技术转移中心有限公司 Preparation method of graphene composite filtering material for efficient integrated water purification equipment for sewage treatment
CN113493963A (en) * 2020-04-01 2021-10-12 苏州合祥纺织科技有限公司 Puerarin-loaded micro-nano composite fiber membrane and preparation method thereof

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CN105483939A (en) * 2016-01-12 2016-04-13 山东佳星环保科技有限公司 Preparation method of porous graphene nanofiber membrane
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KR20160139264A (en) * 2015-05-27 2016-12-07 국방과학연구소 3-dimenstinal nanofiber membrane and Method of manufacturing the same using liquid collector
CN106480552A (en) * 2016-09-28 2017-03-08 广州凯耀资产管理有限公司 Graphene/carbon nano-porous fiber and preparation method and application
CN107868261A (en) * 2017-12-05 2018-04-03 佛山市高明区明城镇新能源新材料产业技术创新中心 A kind of carboxymethyl chitosan/oxidized graphene composite aquogel and its preparation and application

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CN106133213A (en) * 2014-03-28 2016-11-16 高桥光弘 Nano-fiber manufacturing apparatus
KR20160139264A (en) * 2015-05-27 2016-12-07 국방과학연구소 3-dimenstinal nanofiber membrane and Method of manufacturing the same using liquid collector
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110983478A (en) * 2019-11-28 2020-04-10 洪泽联合化纤有限公司 Preparation method of single-component fiber
CN113493963A (en) * 2020-04-01 2021-10-12 苏州合祥纺织科技有限公司 Puerarin-loaded micro-nano composite fiber membrane and preparation method thereof
CN112090169A (en) * 2020-08-12 2020-12-18 柳州紫荆技术转移中心有限公司 Preparation method of graphene composite filtering material for efficient integrated water purification equipment for sewage treatment

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