CN107584138A - Graphene/nano silver nano composite material based on sponge template - Google Patents
Graphene/nano silver nano composite material based on sponge template Download PDFInfo
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- CN107584138A CN107584138A CN201710836768.6A CN201710836768A CN107584138A CN 107584138 A CN107584138 A CN 107584138A CN 201710836768 A CN201710836768 A CN 201710836768A CN 107584138 A CN107584138 A CN 107584138A
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Abstract
The invention discloses a kind of graphene/nano silver nano composite material based on sponge template, using sponge as carrier, pass through electrostatic interaction LBL self-assembly nano-Ag particles and graphene.The present invention guides the three-dimensional macro self assembly of Nano Silver and graphene using business sponge as template, prepares the three-dimensional macro nano structured unit assembly can in sorbing material, photoelectric device, biomedicine field with wide application prospect.
Description
Technical field
The present invention relates to a kind of graphene/nano silver nano composite material based on sponge template, belongs to nano composite material
Field.
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 Silver is a kind of important photoelectric semiconductor material, has wider energy gap at room temperature
（3.37eV）With larger exciton bind energy.Nano Silver has many excellent physical and chemical properties, and such as higher chemistry is steady
It is qualitative, nontoxic and non-migratory, low-k, photocatalysis performance, fluorescence, piezoelectricity, absorb the energy with scatters ultraviolet
Power etc., therefore Nano Silver all has important Research Significance in many fields, and show tempting application prospect.Receive in recent years
Meter Yin is in catalyst, gas sensor, semiconductor devices, piezo-resistance, piezoelectric device, field-emitter display and ultraviolet shading
The fields such as material are 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 carries out dip-coating modification as matrix material, by graphene,
Prepare the polyurethane sponge oil absorption material of super-hydrophobic super-oleophylic；In order to improve stability of the graphene in sponge surface, silicon is utilized
Alkane coupling agent kh-570 is modified to graphene, then is loaded to modified graphene on sponge by dip-coating method, so as to
To the sponge of modified graphene load（The preparation of oleophilic drainage type sponge and film base water-oil separating material and its performance study [D]
Shanghai University, 2016）.
Hunan Normal University is inspired for Yang Xiao days by seashells bio-adhesive albumen, and dopamine is utilized under alkaline environment
Auto polymerization property, in polyurethane sponge surface aggregate activity poly-dopamine thin layer, it is further that silver ion is reduced using glucose
Deposition micro-nano silver particle constructs surface micro-nano structure, and hydrolyzes dimethyl silicone polymer presoma and carry out hydrophobic change to surface
Property, prepare the super hydrophobic surface that contact angle is more than 150 °（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）.North China Electric Power University's Zhai's Wenhua is ground
The general sponge for being loaded with nano silver particles has been studied carefully to Hg in water2+The characterization of adsorption of ion, adsorption conditionses are investigated, found nanometer
Silver-colored sponge has good removal effect to mercury, and saturated adsorption capacity is up to 2.87mg.g-1（Novel nanocomposite materials adsorption and enrichment
Research [D] the North China Electric Power University of mercury species, 2014）.
In addition, also having using sponge as matrix, Fe is assembled3O4Particle, molybdenum disulfide, CNT, titanium dioxide, zinc oxide
Etc. the document report of nano material（On the preparation of oleophilic drainage type sponge and film base water-oil separating material and its performance study [D]
Extra large 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 [D] Harbin Institute of Technology based on the super-hydrophobic sponge of diazonium chemistry, 2016；Artificial lens journal,
2017,46(01):134-138；The preparation of magnetic response polyurethane sponge and oil absorbency research [J] New Chemical Materials,
2017,45(02):239-241；Polyurethane sponge carried titanium dioxide/graphene composite montmorillonoid floating material Visible Light Induced Photocatalytic
17 α-ethinyl estradiol [J] Hohai University's journals (natural science edition), 2017,45 (02):116-121；Super-hydrophobic super parent
The preparation of light wood material and its water-oil separating performance research [D] Northeast Petroleum University, 2016；The system of super infiltration water-oil separating material
Standby and its performance study [D] Jiangsu Universitys, 2016；Chinese invention patent CN201510443105.9 polyurethane sponges load silver
Graphene titanium dioxide nano-particle composite, preparation method and application；Chinese invention patent CN201410170974.4 structures
Make sponge material of zinc oxide fine structure modified polyurethane sponge surface and preparation method thereof；Research of Environmental Sciences, 2016,29
(07):1083-1088；A kind of expanded graphites of Chinese invention patent CN201510470765.6 and the composite modified poly- ammonia of zinc oxide
Ester sponge and preparation method thereof；Chinese invention patent CN201410474510.2 is loaded with the polyurethane sea of hydridization graphite ene coatings
Silk floss and preparation method thereof）.But above-mentioned document relies primarily on the self assembly that dip-coating/dipping means realize nano material, it is this from
Assemble method carries randomness and uncontrollability.
The content of the invention
In view of the above problems, the present invention provides a kind of graphene/nano silver nano composite material based on sponge template.
The technical scheme is that：（1）After sponge is cleaned, square is cut into, is immersed in quality
24h in the sodium dodecyl benzene sulfonate aqueous solution of fraction 1%, bath raio 1:50, vacuum drying after taking-up；（2）Prepare 1-100g/L's
Silver nitrate solution, the 1-100g/L PAMAM aqueous solution is then slowly added into, after ultrasonic mixing is uniform, 80-90 DEG C of reaction 1-12h,
Cleaned repeatedly with ethanol and deionized water, centrifuge, nano-Ag particles are obtained after drying process；（3）By the Nano Silver in step 2
Particle formulation into mass fraction 0.1-5% the aqueous solution, then by the sponge impregnating in step 1 in nano-silver water solution 30-
60min, bath raio 1:10, rinsed, dried repeatedly with deionized water after taking-up；By above-mentioned sponge impregnating in 1-20g/L graphite oxides
30-60min in aqueous solution, bath raio 1:10, rinsed, dried repeatedly with deionized water after taking-up, so far aoxidize stone by one layer
Black alkene/Nano Silver is assembled into the surface of sponge, then repeatedly aforesaid operations, determine as needed sponge surface graphene oxide/
The number of plies of Nano Silver assembling；Finally be placed in reducing agent and reduced, wash, filter, be dried in vacuo after obtain using sponge as mould
The graphene/nano silver composite of plate.
Preferably, the reducing agent is that hydrazine hydrate, sodium borohydride, sodium citrate, vitamin C, hydroiodic acid, tea are more
One or more in phenol.
Compared with prior art, the advantage of the invention is that：Nano Silver and graphene are guided using business sponge as template
Three-dimensional macro self assembly, by the use of the electrostatic interaction between Nano Silver, graphene as film forming motive force, preparing can be in photoelectricity
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 24h in the sodium dodecyl benzene sulfonate aqueous solution of mass fraction 1%,
Bath raio 1:50, vacuum drying after taking-up；（2）1g/L silver nitrate solution is prepared, the PAMAM for being then slowly added into 1g/L is water-soluble
Liquid, after ultrasonic mixing is uniform, 80 DEG C of reaction 1h, is cleaned repeatedly with ethanol and deionized water, centrifuge, nanometer is obtained after drying process
Argent grain；（3）Nano-Ag particles in step 2 are configured to the aqueous solution of mass fraction 0.1%, then by the sea in step 1
Silk floss is immersed in 30min in nano-silver water solution, bath raio 1:10, rinsed, dried repeatedly with deionized water after taking-up；By above-mentioned sponge
It is immersed in 30min in 1g/L graphene oxide water solutions, bath raio 1:10, rinsed, dried, then repeatedly with deionized water after taking-up
90 DEG C of reductase 12 h in hydrazine hydrate solution are placed in, washing, filters, obtain the graphene/nanometer using sponge as template after vacuum drying
Silver composite material.
Embodiment 2
（1）After sponge is cleaned, square is cut into, is immersed in 24h in the sodium dodecyl benzene sulfonate aqueous solution of mass fraction 1%,
Bath raio 1:50, vacuum drying after taking-up；（2）10g/L silver nitrate solution is prepared, the PAMAM for being then slowly added into 10g/L is water-soluble
Liquid, after ultrasonic mixing is uniform, 90 DEG C of reaction 6h, is cleaned repeatedly with ethanol and deionized water, centrifuge, nanometer is obtained after drying process
Argent grain；（3）Nano-Ag particles in step 2 are configured to the aqueous solution of mass fraction 1%, then by the sponge in step 1
It is immersed in 60min in nano-silver water solution, bath raio 1:10, rinsed, dried repeatedly with deionized water after taking-up；Above-mentioned sponge is soaked
Stain 60min in 10g/L graphene oxide water solutions, bath raio 1:10, rinsed, dried, so far repeatedly with deionized water after taking-up
One layer of graphene oxide/Nano Silver has been assembled into the surface of sponge, aforesaid operations has then been repeated twice, is subsequently placed in citric acid
90 DEG C of reduction 12h in sodium, washing, filter, obtain the graphene/nano silver composite using sponge as template after vacuum drying.
Embodiment 3
（1）After sponge is cleaned, square is cut into, is immersed in 24h in the sodium dodecyl benzene sulfonate aqueous solution of mass fraction 1%,
Bath raio 1:50, vacuum drying after taking-up；（2）50g/L silver nitrate solution is prepared, the PAMAM for being then slowly added into 50g/L is water-soluble
Liquid, after ultrasonic mixing is uniform, 90 DEG C of reaction 12h, is cleaned with ethanol and deionized water, centrifuge, received after drying process repeatedly
Rice Argent grain；（3）Nano-Ag particles in step 2 are configured to the aqueous solution of mass fraction 5%, then by the sea in step 1
Silk floss is immersed in 60min in nano-silver water solution, bath raio 1:10, rinsed, dried repeatedly with deionized water after taking-up；By above-mentioned sponge
It is immersed in 60min in 20g/L graphene oxide water solutions, bath raio 1:10, rinsed, dried, extremely repeatedly with deionized water after taking-up
One layer of graphene oxide/Nano Silver has been assembled into the surface of sponge by this, is then repeated four times aforesaid operations, is subsequently placed in boron hydrogen
Change 60 DEG C of reduction 5h in sodium, washing, filter, obtain the graphene/nano silver composite using sponge as template after vacuum drying.
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 (3)
1. using sponge as the graphene/nano silver composite of template, it is characterised in that：
（1）After sponge is cleaned, square is cut into, is immersed in 24h in the sodium dodecyl benzene sulfonate aqueous solution of mass fraction 1%,
Bath raio 1:50, vacuum drying after taking-up；（2）1-100g/L silver nitrate solution is prepared, is then slowly added into 1-100g/L's
The PAMAM aqueous solution, after ultrasonic mixing is uniform, 80-90 DEG C of reaction 1-12h, is cleaned, centrifuged, done repeatedly with ethanol and deionized water
Nano-Ag particles are obtained after dry processing；（3）Nano-Ag particles in step 2 are configured to the mass fraction 0.1-5% aqueous solution,
Then by the sponge impregnating in step 1 in nano-silver water solution 30-60min, bath raio 1:10, it is anti-with deionized water after taking-up
It is multiple to rinse, drying；By above-mentioned sponge impregnating in 1-20g/L graphene oxide water solutions 30-60min, bath raio 1:10, after taking-up
Rinsed, dried repeatedly with deionized water, one layer of graphene oxide/Nano Silver is so far assembled into the surface of sponge, then weight
Multiple aforesaid operations, the number of plies of sponge surface graphene oxide/Nano Silver assembling is determined as needed；Finally it is placed in reducing agent
Row reduction, washing, filter, obtain the graphene/nano silver composite using sponge as template after vacuum drying.
2. the graphene/nano silver nano composite material according to claim 1 based on sponge template, it is characterised in that
The reducing agent is the one or more in hydrazine hydrate, sodium borohydride, sodium citrate, vitamin C, hydroiodic acid, Tea Polyphenols.
3. the graphene/nano silver nano composite material based on sponge template obtained by claim 1 preparation method.
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| CN108832102A (en) * | 2018-06-20 | 2018-11-16 | 青岛大学 | A kind of composite material being used to prepare electrode of lithium cell and its application |
| CN108854261A (en) * | 2018-07-09 | 2018-11-23 | 山东佳星环保科技有限公司 | The preparation method of graphene high-efficiency filtering material for air purifying |
| CN109402839A (en) * | 2018-11-18 | 2019-03-01 | 南通源佑纺织科技有限公司 | A kind of antibacterial polyester fibre lining cloth and its production technology |
| CN110028962A (en) * | 2019-03-18 | 2019-07-19 | 厦门大学 | The preparation method of three-dimensional grapheme and nano silver optical-thermal conversion material based on sponge |
| CN110606981A (en) * | 2019-07-22 | 2019-12-24 | 西交利物浦大学 | Pressure sensor, preparation method and application thereof, and wearable intelligent fabric comprising pressure sensor |
| 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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| CN108832102A (en) * | 2018-06-20 | 2018-11-16 | 青岛大学 | A kind of composite material being used to prepare electrode of lithium cell and its application |
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| CN108854261A (en) * | 2018-07-09 | 2018-11-23 | 山东佳星环保科技有限公司 | The preparation method of graphene high-efficiency filtering material for air purifying |
| CN109402839A (en) * | 2018-11-18 | 2019-03-01 | 南通源佑纺织科技有限公司 | A kind of antibacterial polyester fibre lining cloth and its production technology |
| CN110028962A (en) * | 2019-03-18 | 2019-07-19 | 厦门大学 | The preparation method of three-dimensional grapheme and nano silver optical-thermal conversion material based on sponge |
| CN110606981A (en) * | 2019-07-22 | 2019-12-24 | 西交利物浦大学 | Pressure sensor, preparation method and application thereof, and wearable intelligent fabric comprising pressure sensor |
| CN110606981B (en) * | 2019-07-22 | 2022-03-15 | 西交利物浦大学 | Pressure sensor, preparation method and application thereof, and wearable intelligent fabric comprising pressure sensor |
| 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 |
| CN111333901B (en) * | 2020-03-04 | 2022-09-20 | 上海海事大学 | Flexible composite material and preparation method thereof and method for regulating and controlling negative dielectric property |
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Effective date of registration: 20190717 Address after: 215228, No. 1988, North Ring Road, Shengze, Wujiang District, Jiangsu, Suzhou Patentee after: Jiangsu Hua Hao silk Limited by Share Ltd Address before: 215000 Yuanyao Road, Yuanhe Street, Xiangcheng District, Suzhou City, Jiangsu Province Patentee before: Zhao Bing |