CN107556521A - The three-dimensional porous sponge composite of supported nano zinc oxide - Google Patents
The three-dimensional porous sponge composite of supported nano zinc oxide Download PDFInfo
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- CN107556521A CN107556521A CN201710836746.XA CN201710836746A CN107556521A CN 107556521 A CN107556521 A CN 107556521A CN 201710836746 A CN201710836746 A CN 201710836746A CN 107556521 A CN107556521 A CN 107556521A
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Abstract
The invention discloses a kind of three-dimensional porous sponge composite of supported nano zinc oxide, using sponge as carrier, passes through electrostatic interaction LBL self-assembly nano granular of zinc oxide.The present invention guides the three-dimensional macro self assembly of nano zine oxide using business sponge as template, prepares the three-dimensional macro nano structured unit assembly can in sorbing material, catalysis material, photoelectric device, biomedicine field with wide application prospect.
Description
Technical field
The present invention relates to a kind of three-dimensional porous sponge composite of supported nano zinc oxide, category nano composite material neck
Domain.
Background technology
Inorganic nano material refers to that size is in 1-100nm material, relative to other nano materials, inorganic nano material
With preparing simple, the advantage such as cost is cheap, uniform particle diameter, photocatalysis, solar cell, biology, medicine, weaving, printing and dyeing,
There are extensive research and application in the fields such as wearable electronic.In the inorganic nano material of numerous types, zinc oxide accounts for
According to important position.Nano zine oxide is a kind of important photoelectric semiconductor material, has wider forbidden band wide at room temperature
Degree(3.37eV)With larger exciton bind energy.Nano zine oxide has many excellent physical and chemical properties, as higher
Chemical stability, nontoxic and non-migratory, low-k, photocatalysis performance, fluorescence, piezoelectricity, absorb and scatter ultraviolet
Ability of line etc., therefore nano zine oxide all has important Research Significance in many fields, and before showing tempting application
Scape.Nano zine oxide is in catalyst, gas sensor, semiconductor devices, piezo-resistance, piezoelectric device, field emission in recent years
The field such as display and ultraviolet light screening material is widely used.
In past ten years, researcher is to the assembly research interest more and more higher of nano particle, and they are in nanometer
Substantial amounts of work has been done in terms of one-dimensional, two-dimentional, the three-dimensional self assembly and guide assembling of construction unit.Template is to prepare to receive
The most popular method of rice assembly, it had achieved fast development, but nano structured unit assembly conduct in past 10 years
Design of material and the new technology prepared, it is necessary to it can be accomplished scale production under current process technology and appointed condition, and
This is exactly the difficult point that current template method prepares Nanoscale assemblies.Therefore, also need to simplify assembling flow path, using cheap and easy to get
Mould material, the magnanimity technology of preparing of Nanoscale assemblies is developed, finally realize the practical application of Nanoscale assemblies.
A series of work has been done in this respect by Yu Shuhong seminars of China Science & Technology University.The seminar is with cheap easy
The business sponge obtained is prepared for a series of unit assembly of nanostructureds using sponge as template.They prepare by template of sponge
Gold/cerium dioxide nano line three-dimensional material(Using sponge as the preparation of carrier loaded gold/cerium dioxide nano line three-dimensional material and
It reduces p-nitrophenol (English) [J] Science Bulletin, 2016,61 (09) in continuous-flow system situ:
700-705);Using sponge as macroscopic three dimensional framework template, by simple nano pulp dip-coating means, make nano silver wire
(AgNWs)Under the guide of sponge framework template, the AgNWs three-dimensional macro assemblies with dual-network structure are formed;Using
Nano pulp dipping process, graphene oxide is guided by template of commercial polymer sponge(GO)Three-dimensional assembling, preparation provides
There is the three-dimensional GO macroscopic views assembly of micron order intercommunication pore space structure, corresponding reduced graphene can be obtained after HI acid reduction(RGO)
Three-dimensional macro assembly;Using commercial polymer sponge as template, by nano pulp dipping process, by hydrophobic silica nanometer
Particle(SiO2NPs)And dimethyl silicone polymer(PDMS)The mixture of rubber is coated on the skeleton surface of sponge, is prepared
Porous hydrophobic lipophile material.(The macroscopical Nanoscale assemblies preparation guided based on sponge template and section of application study [D] China
Technology university, 2016).Shanghai University Lee generation generation uses polyurethane(PU)Sponge is carried out as matrix material by graphene
Dip-coating is modified, and prepares the polyurethane sponge oil absorption material of super-hydrophobic super-oleophylic;In order to improve stabilization of the graphene in sponge surface
Property, graphene is modified using Silane coupling reagent KH-570, then modified graphene is loaded to by sponge by dip-coating method
On, so as to obtain the sponge of modified graphene load(The preparation of oleophilic drainage type sponge and film base water-oil separating material and its property
Energy research [D] Shanghai University, 2016).In addition, also have using sponge as matrix, assemble nanometer silver, Fe3O4Particle, molybdenum disulfide,
The document report of the nano materials such as CNT, titanium dioxide(Dimethyl silicone polymer/micro-nano silver/poly-dopamine modification
The preparation of super-hydrophobic sponge and application [J] applied chemistries, 2015,32 (06):726-732;Oleophilic drainage type sponge and film base
The preparation of water-oil separating material and its performance study [D] Shanghai University, 2016;The preparation of super hydrophobic polyurethane (PU) sponge and
Water-oil separating characteristic research [D] Harbin Institute of Technology, 2014;Preparation and sign based on the super-hydrophobic sponge of diazonium chemistry
[D] Harbin Institute of Technology, 2016;Artificial lens journal, 2017,46 (01):134-138;The system of magnetic response polyurethane sponge
Standby and oil absorbency research [J] New Chemical Materials, 2017,45 (02):239-241;Polyurethane sponge carried titanium dioxide/
17 α of graphene composite montmorillonoid floating material Visible Light Induced Photocatalytic-ethinyl estradiol [J] Hohai University journal (natural science
Version), 2017,45 (02):116-121;The preparation of super-hydrophobic super-oleophylic material and its water-oil separating performance research [D] northeast stone
Oily university, 2016;The preparation of super infiltration water-oil separating material and its performance study [D] Jiangsu Universitys, 2016;Chinese invention is special
Sharp CN201510443105.9 polyurethane sponges load silver-colored graphene titanium dioxide nano-particle composite, preparation method and answered
With;Chinese invention patent CN201410170974.4 constructs the sponge material of zinc oxide fine structure modified polyurethane sponge surface
And preparation method thereof).
Specific to zinc oxide, Shanghai University Lee generation generation is modified using micro-nano zinc oxide and palmitic acid and is prepared for super thin
The ZnO-PA modified polyurethane sponges of water super-oleophilic energy(The preparation of oleophilic drainage type sponge and film base water-oil separating material and its
Performance study [D] Shanghai University, 2016).Chemical Engineering institute of Beijing University of Chemical Technology Xu from it is refined using expanded graphite and zinc oxide as
Raw material, using composite modified method modified polyurethane sponge, in the presence of silane coupler, repaiied with lauric alcoholic solution surface
Modified polyurethane sponge is prepared after decorations(Research of Environmental Sciences, 2016,29 (07):1083-1088;Chinese invention patent
A kind of expanded graphites of CN201510470765.6 and the composite modified polyurethane sponge of zinc oxide and preparation method thereof).Middle promulgated by the State Council
Bright patent CN201410474510.2 discloses a kind of polyurethane sponge for being loaded with hydridization graphite ene coatings and preparation method thereof,
The graphite ene coatings of micron zinc oxide hybridization are loaded with polyurethane sponge, the mass ratio of wherein zinc oxide and graphene is
5%.But above-mentioned document relies primarily on the self assembly that dip-coating/dipping means realize nano zine oxide, this self-assembling method carries
Randomness and uncontrollability.
The content of the invention
In view of the above problems, the present invention provides a kind of three-dimensional porous sponge composite of supported nano zinc oxide.
The technical scheme is that:(1)After sponge is cleaned, square is cut into, is immersed in quality
24h in the cationic compound aqueous solution of fraction 1%, bath raio 1:50, vacuum drying after taking-up;(2)Prepare 1mol/L zinc chloride
Solution, 1mol/L sodium hydrate aqueous solution, the volume ratio of the sodium hydroxide solution and liquor zinci chloridi is then added dropwise
For 1:2-2:1, after ultrasonic mixing is uniform, it is slowly added to lauryl sodium sulfate, the lauryl sodium sulfate and zinc chloride
Mass ratio is 1:1-3:1, ultrasonic 2h, move in reactor 160 DEG C of reaction 6-12h, cleaned repeatedly with ethanol and deionized water, from
Zinc oxide nanoparticle is obtained after the heart, drying process;(3)By PAMAM and zinc nitrate hexahydrate be configured to respectively 1-100g/L and
The 1mol/L aqueous solution, the volume ratio of PAMAM and the zinc nitrate hexahydrate aqueous solution is 1:1-5:1, after being mixed evenly,
200 DEG C of reaction 5h in reactor are moved to, cleaned repeatedly with ethanol and deionized water, centrifuge, zinc oxide nano is obtained after drying process
Rice grain;(4)Zinc oxide nanoparticle in step 2 is configured to the mass fraction 0.1-5% aqueous solution, then by step 1
In sponge impregnating in the nano zine oxide aqueous solution 30-60min, bath raio 1:10, rinsed, dried repeatedly with deionized water after taking-up
It is dry;Zinc oxide nanoparticle in step 3 is configured to the mass fraction 0.1-5% aqueous solution, above-mentioned sponge impregnating is being received
30-60min in rice zinc oxide aqueous solution, bath raio 1:10, rinsed, dried, so far by one layer repeatedly with deionized water after taking-up
Nano granular of zinc oxide is assembled into the surface of sponge, and then repeatedly aforesaid operations, decision sponge surface as needed are nano oxidized
The number of plies of zinc assembling.
Preferably, the cationic compound is Hyperbranched Polymer with Terminal Amido, PAMAM, chitosan, divinyl
Triamine, triethylene tetramine, TEPA, poly-dopamine, 2,3- epoxypropyltrimethylchloride chlorides, octyldodecyl diformazan
One or more in ammonium chloride, polyethyleneimine.
Compared with prior art, the advantage of the invention is that:The three of nano zine oxide is guided using business sponge as template
Macroscopical self assembly is tieed up, by the use of the electrostatic interaction between nano zine oxide as film forming motive force, preparing can be in sorbing material, light
Catalysis material, photoelectric device, biomedicine field have the three-dimensional macro nano structured unit assembly of wide application prospect.
Embodiment
The invention will be further elucidated with reference to specific embodiments.
Embodiment 1
(1)After sponge is cleaned, square is cut into, is immersed in the Hyperbranched Polymer with Terminal Amido aqueous solution of mass fraction 1%
24h, bath raio 1:50, vacuum drying after taking-up;(2)1mol/L liquor zinci chloridi is prepared, 1mol/L hydrogen is then added dropwise
Aqueous solution of sodium oxide, the volume ratio of the sodium hydroxide solution and liquor zinci chloridi is 1:2, after ultrasonic mixing is uniform, slowly add
Enter lauryl sodium sulfate, the mass ratio of the lauryl sodium sulfate and zinc chloride is 1:1, ultrasonic 2h, move in reactor
160 DEG C of reaction 6h, are cleaned, centrifuge, Zinc oxide nanoparticle are obtained after drying process repeatedly with ethanol and deionized water;(3)Will
PAMAM and zinc nitrate hexahydrate are configured to 1g/L and the 1mol/L aqueous solution respectively, and the PAMAM and zinc nitrate hexahydrate are water-soluble
The volume ratio of liquid is 1:1, after being mixed evenly, 200 DEG C of reaction 5h are moved in reactor, it is repeatedly clear with ethanol and deionized water
Wash, centrifuge, Zinc oxide nanoparticle is obtained after drying process;(4)Zinc oxide nanoparticle in step 2 is configured to quality
The aqueous solution of fraction 0.1%, then by the sponge impregnating in step 1 in the nano zine oxide aqueous solution 30min, bath raio 1:10,
Rinsed, dried repeatedly with deionized water after taking-up;Zinc oxide nanoparticle in step 3 is configured to mass fraction 0.1%
The aqueous solution, by above-mentioned sponge impregnating in the nano zine oxide aqueous solution 30min, bath raio 1:10, after taking-up with deionized water repeatedly
Rinse, drying, obtain the three-dimensional porous sponge composite of supported nano zinc oxide.
Embodiment 2
(1)After sponge is cleaned, square is cut into, is immersed in 24h in the aq. polyethyleneimine of mass fraction 1%, bath raio 1:
50, vacuum drying after taking-up;(2)1mol/L liquor zinci chloridi is prepared, the sodium hydroxide that 1mol/L is then added dropwise is water-soluble
Liquid, the volume ratio of the sodium hydroxide solution and liquor zinci chloridi is 1:1, after ultrasonic mixing is uniform, it is slowly added to dodecyl
The mass ratio of sodium sulphate, the lauryl sodium sulfate and zinc chloride is 2:1, ultrasonic 2h, move to 160 DEG C of reactions in reactor
9h, cleaned repeatedly with ethanol and deionized water, centrifuge, Zinc oxide nanoparticle is obtained after drying process;(3)By PAMAM and six
Nitric hydrate zinc is configured to 10g/L and the 1mol/L aqueous solution, the volume of PAMAM and the zinc nitrate hexahydrate aqueous solution respectively
Than for 2:1, after being mixed evenly, 200 DEG C of reaction 5h in reactor are moved to, cleaned, centrifuged repeatedly with ethanol and deionized water,
Zinc oxide nanoparticle is obtained after drying process;(4)Zinc oxide nanoparticle in step 2 is configured to mass fraction 1%
The aqueous solution, then by the sponge impregnating in step 1 in the nano zine oxide aqueous solution 50min, bath raio 1:10, spent after taking-up
Ionized water rinses repeatedly, drying;Zinc oxide nanoparticle in step 3 is configured to the aqueous solution of mass fraction 1%, will be above-mentioned
Sponge impregnating 50min in the nano zine oxide aqueous solution, bath raio 1:10, rinsed, dried, so far repeatedly with deionized water after taking-up
One layer of nano granular of zinc oxide has been assembled into the surface of sponge, has then been repeated once aforesaid operations, has obtained loading nano oxidized
The three-dimensional porous sponge composite of zinc.
Embodiment 3
(1)After sponge is cleaned, square is cut into, 2, the 3- epoxypropyltrimethylchloride chlorides for being immersed in mass fraction 1% are water-soluble
24h in liquid, bath raio 1:50, vacuum drying after taking-up;(2)1mol/L liquor zinci chloridi is prepared, 1mol/L is then added dropwise
Sodium hydrate aqueous solution, the volume ratio of the sodium hydroxide solution and liquor zinci chloridi is 2:1, after ultrasonic mixing is uniform, delay
The mass ratio of slow addition lauryl sodium sulfate, the lauryl sodium sulfate and zinc chloride is 3:1, ultrasonic 2h, move to reaction
160 DEG C of reaction 12h, are cleaned, centrifuge, Zinc oxide nanoparticle are obtained after drying process repeatedly with ethanol and deionized water in kettle;
(3)PAMAM and zinc nitrate hexahydrate are configured to 20g/L and the 1mol/L aqueous solution, the PAMAM and six nitric hydrates respectively
The volume ratio of the zinc aqueous solution is 5:1, after being mixed evenly, 200 DEG C of reaction 5h in reactor are moved to, with ethanol and deionized water
Clean repeatedly, centrifuge, obtain Zinc oxide nanoparticle after drying process;(4)Zinc oxide nanoparticle in step 2 is prepared
Into the aqueous solution of mass fraction 5%, then by the sponge impregnating in step 1 in the nano zine oxide aqueous solution 60min, bath raio 1:
10, rinsed, dried repeatedly with deionized water after taking-up;Zinc oxide nanoparticle in step 3 is configured to mass fraction 5%
The aqueous solution, by above-mentioned sponge impregnating in the nano zine oxide aqueous solution 60min, bath raio 1:10, after taking-up with deionized water repeatedly
Rinse, drying, one layer of nano granular of zinc oxide is so far assembled into the surface of sponge, aforesaid operations is then repeated twice, obtains
To the three-dimensional porous sponge composite of supported nano zinc oxide.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention.For those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms.Here all embodiments can not be exhaustive.It is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is amplified out still in protection scope of the present invention.
Claims (6)
1. the three-dimensional porous sponge composite of supported nano zinc oxide, it is characterised in that:Cationic compound is pretreated
Sponge as carrier, pass through electrostatic interaction LBL self-assembly nano granular of zinc oxide;
Preparation process is as follows:(1)After sponge is cleaned, square is cut into, is immersed in the cationic compound water of mass fraction 1%
24h in solution, bath raio 1:50, vacuum drying after taking-up;(2)1mol/L liquor zinci chloridi is prepared, 1mol/ is then added dropwise
L sodium hydrate aqueous solution, after ultrasonic mixing is uniform, lauryl sodium sulfate is slowly added to, ultrasonic 2h, is moved in reactor
160 DEG C of reaction 6-12h, are cleaned, centrifuge, Zinc oxide nanoparticle are obtained after drying process repeatedly with ethanol and deionized water;(3)
PAMAM and zinc nitrate hexahydrate are configured to 1-100g/L and the 1mol/L aqueous solution respectively, after being mixed evenly, moved to anti-
200 DEG C of reaction 5h in kettle are answered, cleaned repeatedly with ethanol and deionized water, centrifuge, Zinc oxide nanoparticle is obtained after drying process;
(4)Zinc oxide nanoparticle in step 2 is configured to the mass fraction 0.1-5% aqueous solution, then by the sea in step 1
Silk floss is immersed in 30-60min in the nano zine oxide aqueous solution, bath raio 1:10, rinsed, dried repeatedly with deionized water after taking-up;Will
Zinc oxide nanoparticle in step 3 is configured to the mass fraction 0.1-5% aqueous solution, by above-mentioned sponge impregnating nano oxidized
30-60min in the zinc aqueous solution, bath raio 1:10, rinsed, dried, so far by one layer of nano oxygen repeatedly with deionized water after taking-up
Change the surface that zinc particle is assembled into sponge, then repeatedly aforesaid operations, decision sponge surface nano zine oxide as needed assemble
The number of plies.
2. the three-dimensional porous sponge composite of supported nano zinc oxide according to claim 1, it is characterised in that described
Cationic compound is Hyperbranched Polymer with Terminal Amido, PAMAM, chitosan, diethylenetriamine, triethylene tetramine, four ethene five
In amine, poly-dopamine, 2,3- epoxypropyltrimethylchloride chlorides, octyldodecyl alkyl dimethyl ammonium chloride, polyethyleneimine
It is one or more.
3. the three-dimensional porous sponge composite of supported nano zinc oxide according to claim 1, it is characterised in that described
The volume ratio of sodium hydroxide solution and liquor zinci chloridi is 1:2-2:1.
4. the three-dimensional porous sponge composite of supported nano zinc oxide according to claim 1, it is characterised in that described
The mass ratio of lauryl sodium sulfate and zinc chloride is 1:1-3:1.
5. the three-dimensional porous sponge composite of supported nano zinc oxide according to claim 1, it is characterised in that described
The volume ratio of PAMAM and the zinc nitrate hexahydrate aqueous solution is 1:1-5:1.
6. the three-dimensional porous sponge composite of the supported nano zinc oxide obtained by claim 1 preparation method.
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Cited By (5)
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CN110394196A (en) * | 2019-07-05 | 2019-11-01 | 广西大学 | A kind of preparation method of nano-titanium dioxide-polyurethane sponge composite material |
CN110444730A (en) * | 2019-08-19 | 2019-11-12 | 中南大学 | A kind of preparation method and application of tridimensional network nanometer layer zinc load |
CN110823396A (en) * | 2018-08-08 | 2020-02-21 | 中国科学院苏州纳米技术与纳米仿生研究所 | Temperature sensor based on reduced graphene oxide and preparation method and application thereof |
CN111333901A (en) * | 2020-03-04 | 2020-06-26 | 上海海事大学 | Flexible composite material and preparation method thereof and method for regulating negative dielectric property |
CN113019345A (en) * | 2021-04-20 | 2021-06-25 | 福州大学 | Sponge-based composite absorbent for low-concentration organic solvent wastewater treatment and preparation method and application thereof |
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CN106389388A (en) * | 2016-11-10 | 2017-02-15 | 苏州大学 | PH redox double-sensitive PAMAM targeting nano drug delivery carrier and preparation method thereof |
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CN105413672A (en) * | 2015-11-25 | 2016-03-23 | 天津中材工程研究中心有限公司 | Nano-zinc oxide and carbon fiber composite material and preparation method thereof |
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Cited By (6)
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CN110823396A (en) * | 2018-08-08 | 2020-02-21 | 中国科学院苏州纳米技术与纳米仿生研究所 | Temperature sensor based on reduced graphene oxide and preparation method and application thereof |
CN110394196A (en) * | 2019-07-05 | 2019-11-01 | 广西大学 | A kind of preparation method of nano-titanium dioxide-polyurethane sponge composite material |
CN110444730A (en) * | 2019-08-19 | 2019-11-12 | 中南大学 | A kind of preparation method and application of tridimensional network nanometer layer zinc load |
CN111333901A (en) * | 2020-03-04 | 2020-06-26 | 上海海事大学 | Flexible composite material and preparation method thereof and method for regulating negative dielectric property |
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CN113019345A (en) * | 2021-04-20 | 2021-06-25 | 福州大学 | Sponge-based composite absorbent for low-concentration organic solvent wastewater treatment and preparation method and application thereof |
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