CN110485157A - Chitosan graft mesoporous silicon dioxide nano tunica fibrosa preparation method and applications - Google Patents
Chitosan graft mesoporous silicon dioxide nano tunica fibrosa preparation method and applications Download PDFInfo
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- CN110485157A CN110485157A CN201910709804.1A CN201910709804A CN110485157A CN 110485157 A CN110485157 A CN 110485157A CN 201910709804 A CN201910709804 A CN 201910709804A CN 110485157 A CN110485157 A CN 110485157A
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- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- 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
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- 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
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
- B01J20/28038—Membranes or mats made from fibers or filaments
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- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/305—Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores
- B01J20/3057—Use of a templating or imprinting material ; filling pores of a substrate or matrix followed by the removal of the substrate or matrix
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- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/305—Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores
- B01J20/3064—Addition of pore forming agents, e.g. pore inducing or porogenic agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING 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
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
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- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The present invention is chitosan graft mesoporous silicon dioxide nano tunica fibrosa preparation method and applications, for adsorbing the heavy metal material in water.The present invention is using polyvinyl alcohol and ethyl orthosilicate (TEOS) hydrolyzate as spinning solution, and electrostatic spinning obtains nano fibrous membrane, and tunica fibrosa is placed in Muffle furnace and is calcined, the silica nano fibrous membrane for the polyvinyl alcohol that is removed.After fiber film surface is coated epoxy silane coupling agent KH-560, it is dipped in 10h in the dispersion liquid of the acetone of chitosan, obtains the silica nano fibrous membrane of surface grafting chitosan.Present invention process is simple, easily operated, gained nano fibrous membrane large specific surface area, can be recycled and recycles, and has mesoporous silicon oxide and the dual absorption of chitosan, can effectively adsorb the heavy metal ion in water, have broad prospects in terms of water process.
Description
Technical field
The invention belongs to functional materials and field of environment engineering, and in particular to chitosan graft mesoporous silicon dioxide nano is fine
Tie up the preparation of film.
Background technique
With the development that deepens continuously of global industry, water pollution becomes serious environmental problem, contains not in waste water
Degradable heavy metal, toxicity is big, easily assembles, destructive to ecological environmental pollution very big, causes the extensive concern of people.These
Heavy metal ion can enter human body by food chain, cannot be discharged, and after human body enrichment, may result in gene mutation and then increase
Add the risk for suffering from cancer.In addition, heavy metal ion has serious damage to the digestive system and nervous system of human body, make human body
Immunocompetence decline, is detrimental to health.Therefore, effectively removing heavy metal ion in water becomes very urgent.
The minimizing technology of Heavy Metals in Waters mainly has chemical precipitation method, graphene absorption, ion exchange, electrochemistry at present
Method, oxidation-reduction method and liquid-film method.Chemical precipitation method there are secondary pollution, at high cost, treatment effeciency is low；Graphene adsorbs cost
Higher, recycling difficulty；Ion exchange energy consumption height, resin are easily by high-valence state metal Oxidative inactivation；Electrochemical process wastewater treatment capacity is small,
Treatment effeciency is low, at high cost；Oxidation-reduction method, specific oxidant increase cost；Condensate film stability is poor, service life is short.Cause
This exploitation is cheap, and the high heavy metal ion adsorbing material of adsorption efficiency becomes research hotspot in recent years.Electrostatic spinning is received
Rice fiber is used for the heavy metal ion adsorbed in water and widely was studied in recent years, because of its large specific surface area, preparation simply, at
Sheet is cheap, is easily isolated the advantages that good with reusable performance, the extensive concern by scientific research personnel.
Mesoporous silicon oxide in bulky molecular catalysis, is received due to having many advantages, such as high-specific surface area, regular cellular structure
Rice reactor and adsorbing separation etc. have broad application prospects.The silica nano fibrous membrane of electrostatic spinning preparation
Specific surface is greatly improved, so that increasing with heavy metal ion contact area, effectively improves adsorption efficiency.Chitosan point
Son has a large amount of amino and hydroxyl because its skeleton is longer, chelation can occur with heavy metal ion, become excellent weight
Metal absorbent, but because chitosan is pulverulent solids, it is not easily recycled, its application is made to receive limitation.
Summary of the invention
The purpose of the present invention is being directed to Heavy Metals in Water Environment ion contamination problems, it is mesoporous to propose a kind of chitosan graft
The preparation method of silica nano fibrous membrane.The present invention utilizes a large amount of in the mesoporous absorption and chitosan molecule chain of silica
The absorption of amino and hydroxyl combines, and achievees the effect that dual absorption, greatly improves adsorption efficiency, mechanical performance and stabilization
Property improve and solve adsorbent material recycling difficult problem.
The technical solution adopted by the invention is as follows:
Chitosan graft mesoporous silicon dioxide nano tunica fibrosa, that is, electrostatic spinning prepares silica nano fibrous membrane, passes through
Epoxy silane coupling agent KH-560 is by chitosan graft on silicon dioxide fibre surface.
The preparation method of chitosan graft mesoporous silicon dioxide nano tunica fibrosa, comprising the following steps:
(1) preparation of PVA aqueous solution: weighing appropriate PVA, be slowly added to while stirring, after being swollen half an hour, heating stirring
It is dissolved sufficiently to 80 DEG C；
(2) prepared by TEOS hydrolyzate: weighing TEOS, water and cetyl trimethylammonium bromide (CTAB) in proportion, then
It takes appropriate NaOH that reagent bottle is added, stirs 12h under room temperature, configured TEOS hydrolyzate；
(3) PVA aqueous solution and TEOS hydrolyzate are weighed to mixing 10h in mass ratio, spinning solution is prepared, be
Increase spinnability, is added appropriate NaCl, later, injects in syringe and carries out electrostatic spinning, obtain PVA-SiO2Nanofiber
Film；
(4) obtained tunica fibrosa is placed in Muffle furnace to calcine, removes polyvinyl alcohol and CTAB, obtains meso-porous titanium dioxide
Silicon nanofiber
(5) finally coat one layer of epoxy silane coupling agent KH-560 in obtained fiber film surface, be placed on chitosan
Acetone dispersion liquor in stir 10h, take out drying.
Preferably, PVA mass fraction is 20% in the step (1).
Preferably, TESO in the step (2): water: CTAB mass ratio is 1:8.1:0.1, water: NaOH 1:0.001.
Preferably, PVA aqueous solution and TEOS hydrolyzate mass ratio are 1:1,1:2,2:1 in the step (3), it is added molten
The mass fraction of liquid is the NaCl of 0.5wt%.The high voltage power supply output voltage of spinning is 20KV, and spinning solution flow velocity is 0.6mL/
H, distance is 20cm between reception device and spinning nozzle.
Preferably, Muffle furnace heating rate is 5 DEG C/min in the step (4), temperature is 800 DEG C.
Preferably, the concentration of chitosan is 1wt%, 2wt% and 3wt%. in the step (5)
Chitosan graft mesoporous silicon dioxide nano tunica fibrosa, the application as absorbing heavy metal ions in water.
The application of chitosan graft mesoporous silicon dioxide nano tunica fibrosa of the invention in absorption heavy metal ion, therewith
Preceding pertinent literature report is compared, and is had the advantage that
(1) chitosan graft mesoporous silicon dioxide nano tunica fibrosa of the invention, electrostatic spinning prepare silica nanometer
Tunica fibrosa can significantly improve spinnability using template polymer PVA, and fine using the silica nanometer of PVA system preparation
Tieing up film has preferably flexible and mechanical performance.Pore creating material and template are removed simultaneously after Muffle furnace sintering, prepares meso-porous titanium dioxide
Silicon nano fibrous membrane, surface area increase, and the contact area of the heavy metal ion in water and tunica fibrosa can be significantly greatly increased, and improve and inhale
Attached efficiency；
(2) chitosan graft mesoporous silicon dioxide nano tunica fibrosa of the invention, chitosan are grafted using silane coupling agent
Amino and hydroxyl on fiber surface, chitosan skeleton can generate chelation in metal ion, with mesoporous silicon oxide
Synergistic effect is played, effective suction-operated is played to the heavy metal ion in water；
(3) chitosan graft mesoporous silicon dioxide nano tunica fibrosa of the invention, is able to solve chitosan as adsorption material
The shortcomings that material is not easily recycled, so that save the cost, recycles material.
Detailed description of the invention
Fig. 1 is that electrostatic spinning of the present invention tests easy device figure；
Fig. 2 is the scanning electron microscope (SEM) photograph of the mesoporous silicon dioxide nano tunica fibrosa of this experiment synthesis；
Specific embodiment
The synthetic example of PVA aqueous solution and the preparation of TEOS hydrolyzate:
(1) preparation of PVA aqueous solution: configuring 20% PVA aqueous solution, be slowly added in water while stirring after weighing PVA,
After being swollen half an hour, heating, which is stirred to 80 DEG C, dissolves it sufficiently；
(2) prepared by TEOS hydrolyzate: weighing TEOS, water and cetyl trimethyl bromine by the mass ratio of 1:8.1:0.1
Change ammonium (CTAB), then weigh water: reagent bottle is added in the NaOH that the ratio of NaOH is 1:0.001, stirs 12h under room temperature, configures
Good TEOS hydrolyzate.
Embodiment 1
10h is mixed by the mass ratio of 1:1 in PVA aqueous solution and TEOS hydrolyzate, spinning solution is prepared, in order to
Increase spinnability, the NaCl of 0.5wt% is added, later, injects in syringe and carry out electrostatic spinning, the high voltage power supply output of spinning
Voltage is 20KV, and spinning solution flow velocity is 0.6mL/h, and distance is 20cm between reception device and spinning nozzle, obtains PVA-SiO2
Nano fibrous membrane.
It is 5 DEG C/min that obtained tunica fibrosa, which is placed in Muffle furnace heating rate, and temperature is 800 DEG C and is calcined, and is removed poly-
Vinyl alcohol and CTAB obtain mesoporous silicon dioxide nano fiber
Finally coat one layer of epoxy silane coupling agent KH-560 in obtained fiber film surface, to be placed on 1wt% shell poly-
10h is stirred in the acetic acid solution of sugar, takes out drying.
Embodiment 2
10h is mixed by the mass ratio of 1:1 in PVA aqueous solution and TEOS hydrolyzate, spinning solution is prepared, in order to
Increase spinnability, the NaCl of 0.5wt% is added, later, injects in syringe and carry out electrostatic spinning, the high voltage power supply output of spinning
Voltage is 20KV, and spinning solution flow velocity is 0.6mL/h, and distance is 20cm between reception device and spinning nozzle, obtains PVA-SiO2
Nano fibrous membrane.
It is 5 DEG C/min that obtained tunica fibrosa, which is placed in Muffle furnace heating rate, and temperature is 800 DEG C and is calcined, and is removed poly-
Vinyl alcohol and CTAB obtain mesoporous silicon dioxide nano fiber
Finally coat one layer of epoxy silane coupling agent KH-560 in obtained fiber film surface, to be placed on 2wt% shell poly-
10h is stirred in the acetic acid solution of sugar, takes out drying.
Embodiment 3
10h is mixed by the mass ratio of 1:1 in PVA aqueous solution and TEOS hydrolyzate, spinning solution is prepared, in order to
Increase spinnability, the NaCl of 0.5wt% is added, later, injects in syringe and carry out electrostatic spinning, the high voltage power supply output of spinning
Voltage is 20KV, and spinning solution flow velocity is 0.6mL/h, and distance is 20cm between reception device and spinning nozzle, obtains PVA-SiO2
Nano fibrous membrane.
It is 5 DEG C/min that obtained tunica fibrosa, which is placed in Muffle furnace heating rate, and temperature is 800 DEG C and is calcined, and is removed poly-
Vinyl alcohol and CTAB obtain mesoporous silicon dioxide nano fiber
Finally coat one layer of epoxy silane coupling agent KH-560 in obtained fiber film surface, to be placed on 3wt% shell poly-
10h is stirred in the acetic acid solution of sugar, takes out drying.
Embodiment 4
10h is mixed by the mass ratio of 1:2 in PVA aqueous solution and TEOS hydrolyzate, spinning solution is prepared, in order to
Increase spinnability, the NaCl of 0.5wt% is added, later, injects in syringe and carry out electrostatic spinning, the high voltage power supply output of spinning
Voltage is 20KV, and spinning solution flow velocity is 0.6mL/h, and distance is 20cm between reception device and spinning nozzle, obtains PVA-SiO2
Nano fibrous membrane.
It is 5 DEG C/min that obtained tunica fibrosa, which is placed in Muffle furnace heating rate, and temperature is 800 DEG C and is calcined, and is removed poly-
Vinyl alcohol and CTAB obtain mesoporous silicon dioxide nano fiber
Finally coat one layer of epoxy silane coupling agent KH-560 in obtained fiber film surface, to be placed on 1wt% shell poly-
10h is stirred in the acetic acid solution of sugar, takes out drying.
Embodiment 5
10h is mixed by the mass ratio of 1:2 in PVA aqueous solution and TEOS hydrolyzate, spinning solution is prepared, in order to
Increase spinnability, the NaCl of 0.5wt% is added, later, injects in syringe and carry out electrostatic spinning, the high voltage power supply output of spinning
Voltage is 20KV, and spinning solution flow velocity is 0.6mL/h, and distance is 20cm between reception device and spinning nozzle, obtains PVA-SiO2
Nano fibrous membrane.
It is 5 DEG C/min that obtained tunica fibrosa, which is placed in Muffle furnace heating rate, and temperature is 800 DEG C and is calcined, and is removed poly-
Vinyl alcohol and CTAB obtain mesoporous silicon dioxide nano fiber
Finally coat one layer of epoxy silane coupling agent KH-560 in obtained fiber film surface, to be placed on 2wt% shell poly-
10h is stirred in the acetic acid solution of sugar, takes out drying.
Embodiment 6
10h is mixed by the mass ratio of 1:2 in PVA aqueous solution and TEOS hydrolyzate, spinning solution is prepared, in order to
Increase spinnability, the NaCl of 0.5wt% is added, later, injects in syringe and carry out electrostatic spinning, the high voltage power supply output of spinning
Voltage is 20KV, and spinning solution flow velocity is 0.6mL/h, and distance is 20cm between reception device and spinning nozzle, obtains PVA-SiO2
Nano fibrous membrane.
It is 5 DEG C/min that obtained tunica fibrosa, which is placed in Muffle furnace heating rate, and temperature is 800 DEG C and is calcined, and is removed poly-
Vinyl alcohol and CTAB obtain mesoporous silicon dioxide nano fiber
Finally coat one layer of epoxy silane coupling agent KH-560 in obtained fiber film surface, to be placed on 3wt% shell poly-
10h is stirred in the acetic acid solution of sugar, takes out drying.
Embodiment 7
10h is mixed by the mass ratio of 2:1 in PVA aqueous solution and TEOS hydrolyzate, spinning solution is prepared, in order to
Increase spinnability, the NaCl of 0.5wt% is added, later, injects in syringe and carry out electrostatic spinning, the high voltage power supply output of spinning
Voltage is 20KV, and spinning solution flow velocity is 0.6mL/h, and distance is 20cm between reception device and spinning nozzle, obtains PVA-SiO2
Nano fibrous membrane.
It is 5 DEG C/min that obtained tunica fibrosa, which is placed in Muffle furnace heating rate, and temperature is 800 DEG C and is calcined, and is removed poly-
Vinyl alcohol and CTAB obtain mesoporous silicon dioxide nano fiber
Finally coat one layer of epoxy silane coupling agent KH-560 in obtained fiber film surface, to be placed on 1wt% shell poly-
10h is stirred in the acetic acid solution of sugar, takes out drying.
Embodiment 8
10h is mixed by the mass ratio of 2:1 in PVA aqueous solution and TEOS hydrolyzate, spinning solution is prepared, in order to
Increase spinnability, the NaCl of 0.5wt% is added, later, injects in syringe and carry out electrostatic spinning, the high voltage power supply output of spinning
Voltage is 20KV, and spinning solution flow velocity is 0.6mL/h, and distance is 20cm between reception device and spinning nozzle, obtains PVA-SiO2
Nano fibrous membrane.
It is 5 DEG C/min that obtained tunica fibrosa, which is placed in Muffle furnace heating rate, and temperature is 800 DEG C and is calcined, and is removed poly-
Vinyl alcohol and CTAB obtain mesoporous silicon dioxide nano fiber
Finally coat one layer of epoxy silane coupling agent KH-560 in obtained fiber film surface, to be placed on 2wt% shell poly-
10h is stirred in the acetic acid solution of sugar, takes out drying.
Embodiment 9
10h is mixed by the mass ratio of 2:1 in PVA aqueous solution and TEOS hydrolyzate, spinning solution is prepared, in order to
Increase spinnability, the NaCl of 0.5wt% is added, later, injects in syringe and carry out electrostatic spinning, the high voltage power supply output of spinning
Voltage is 20KV, and spinning solution flow velocity is 0.6mL/h, and distance is 20cm between reception device and spinning nozzle, obtains PVA-SiO2
Nano fibrous membrane.
It is 5 DEG C/min that obtained tunica fibrosa, which is placed in Muffle furnace heating rate, and temperature is 800 DEG C and is calcined, and is removed poly-
Vinyl alcohol and CTAB obtain mesoporous silicon dioxide nano fiber
Finally coat one layer of epoxy silane coupling agent KH-560 in obtained fiber film surface, to be placed on 3wt% shell poly-
10h is stirred in the acetic acid solution of sugar, takes out drying.
Application Example
Adsorption experiment: using containing Cu2+、Ni2+、Cr2+Chitosan graft mesoporous silicon oxide is tested with the waste water solution of Fe2+
The adsorption efficiency experiment of nano fibrous membrane PH under different time and difference.
Claims (8)
1. chitosan graft mesoporous silicon dioxide nano tunica fibrosa, that is, electrostatic spinning prepares silica nano fibrous membrane, pass through ring
Oxosilane coupling agent KH-560 is by chitosan graft on silicon dioxide fibre surface.
2. the preparation method of chitosan graft mesoporous silicon dioxide nano tunica fibrosa, comprising the following steps:
(1) preparation of PVA aqueous solution: weighing appropriate PVA, be slowly added to while stirring, after being swollen half an hour, heating stirring to 80
DEG C dissolve it sufficiently；
(2) prepared by TEOS hydrolyzate: weighing TEOS, water and cetyl trimethylammonium bromide (CTAB) in proportion, then takes suitable
It measures NaOH and reagent bottle is added, stir 12h under room temperature, configured TEOS hydrolyzate；
(3) PVA aqueous solution and TEOS hydrolyzate are weighed to mixing 10h in mass ratio, spinning solution is prepared, in order to increase
Add spinnability, appropriate NaCl is added, later, injects in syringe and carry out electrostatic spinning, obtain PVA-SiO2Nano fibrous membrane；
(4) obtained tunica fibrosa is placed in Muffle furnace to calcine, removes polyvinyl alcohol and CTAB, obtains mesoporous silicon oxide and receive
Rice fiber；
(5) finally coat one layer of epoxy silane coupling agent KH-560 in obtained fiber film surface, the second for being placed on chitosan
10h is stirred in acid solution, takes out drying.
3. preparation method according to claim 2, it is characterised in that: PVA mass fraction is 20% in the step (1).
4. preparation method according to claim 2, it is characterised in that: TESO in the step (2): water: CTAB mass ratio
For 1:8.1:0.1.
5. preparation method according to claim 2, it is characterised in that: PVA aqueous solution and TEOS hydrolysis in the step (3)
Liquid mass ratio is 1:1,1:2,2:1, and the mass fraction that solution is added is the NaCl of 0.5wt%, and the high voltage power supply of spinning exports electricity
Pressure is 20KV, and spinning solution flow velocity is 0.6mL/h, and distance is 20cm between reception device and spinning nozzle.
6. preparation method according to claim 2, it is characterised in that: Muffle furnace heating rate is 5 in the step (4)
DEG C/min, temperature is 800 DEG C.
7. preparation method according to claim 2, it is characterised in that: the concentration of chitosan is in the step (5)
1wt%, 2wt% and 3wt%.
8. the application of chitosan graft mesoporous silicon dioxide nano tunica fibrosa prepared by claim 2, it is characterised in that: as
Adsorb the application of heavy metal ion material.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111411509A (en) * | 2020-05-08 | 2020-07-14 | 安徽省农业科学院棉花研究所 | Nano chitosan modified cotton fiber and preparation method thereof |
| CN111821954A (en) * | 2020-07-25 | 2020-10-27 | 合肥学院 | Preparation method and application of hybrid membrane adsorbent for removing nickel ions in water |
| CN112275288A (en) * | 2020-09-21 | 2021-01-29 | 郑州大学 | Preparation method and application of copper-cobalt oxide-loaded carbon nanofiber composite material |
| CN112473630A (en) * | 2020-11-13 | 2021-03-12 | 山东东岳化工有限公司 | Composite graphene chitosan aerogel and preparation method and application thereof |
| CN113185874A (en) * | 2021-05-14 | 2021-07-30 | 胡召锦 | Oil-stain-resistant self-cleaning coating and preparation method thereof |
| CN114653334A (en) * | 2022-03-15 | 2022-06-24 | 广西大学 | Bi synthesized by hydrothermal method2S3@SiO2Nanofiber membrane and preparation method and application thereof |
| CN115595784A (en) * | 2022-09-27 | 2023-01-13 | 中国海洋大学（Cn） | Composite chitosan preservative film and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111411509A (en) * | 2020-05-08 | 2020-07-14 | 安徽省农业科学院棉花研究所 | Nano chitosan modified cotton fiber and preparation method thereof |
| CN111821954A (en) * | 2020-07-25 | 2020-10-27 | 合肥学院 | Preparation method and application of hybrid membrane adsorbent for removing nickel ions in water |
| CN112275288A (en) * | 2020-09-21 | 2021-01-29 | 郑州大学 | Preparation method and application of copper-cobalt oxide-loaded carbon nanofiber composite material |
| CN112275288B (en) * | 2020-09-21 | 2023-04-14 | 郑州大学 | Preparation method and application of copper-cobalt oxide loaded carbon nanofiber composite material |
| CN112473630A (en) * | 2020-11-13 | 2021-03-12 | 山东东岳化工有限公司 | Composite graphene chitosan aerogel and preparation method and application thereof |
| CN113185874A (en) * | 2021-05-14 | 2021-07-30 | 胡召锦 | Oil-stain-resistant self-cleaning coating and preparation method thereof |
| CN113185874B (en) * | 2021-05-14 | 2022-05-06 | 浙江鱼童新材料股份有限公司 | Oil-stain-resistant self-cleaning coating and preparation method thereof |
| CN114653334A (en) * | 2022-03-15 | 2022-06-24 | 广西大学 | Bi synthesized by hydrothermal method2S3@SiO2Nanofiber membrane and preparation method and application thereof |
| CN114653334B (en) * | 2022-03-15 | 2023-08-04 | 广西大学 | Bi synthesized by hydrothermal method 2 S 3 @SiO 2 Nanofiber membrane and preparation method and application thereof |
| CN115595784A (en) * | 2022-09-27 | 2023-01-13 | 中国海洋大学（Cn） | Composite chitosan preservative film and preparation method thereof |
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