CN107584138B - Graphene/nano silver nanocomposite based on sponge template - Google Patents
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- CN107584138B CN107584138B CN201710836768.6A CN201710836768A CN107584138B CN 107584138 B CN107584138 B CN 107584138B CN 201710836768 A CN201710836768 A CN 201710836768A CN 107584138 B CN107584138 B CN 107584138B
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Abstract
The invention discloses a kind of graphene/nano silver nanocomposites based on sponge template to pass through electrostatic interaction LBL self-assembly nano-Ag particles and graphene using sponge as carrier.The present invention guides the three-dimensional macro self assembly of nano silver and graphene using business sponge as template, and preparing can be in the three-dimensional macro nano structured unit assembly of adsorbent material, photoelectric device, biomedicine field with wide application prospect.
Description
Technical field
The present invention relates to a kind of graphene/nano silver nanocomposites based on sponge template, belong to nanocomposite
Field.
Background technique
Inorganic nano material refers to that size is in the material of 1-100nm, relative to other nano materials, inorganic nano material
Simple, the advantages such as low in cost, uniform particle diameter with preparation, photocatalysis, solar battery, 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 is accounted for
According to important position.Nano silver is a kind of important photoelectric semiconductor material, has wider forbidden bandwidth at room temperature
(3.37eV) and biggish 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, the energy of absorption and scatters ultraviolet
Power etc., therefore nano silver all has important research significance in many fields, and shows tempting application prospect.It receives in recent years
Meter Yin is in catalyst, gas sensor, semiconductor devices, varistor, piezoelectric device, field-emitter display and ultraviolet shading
The fields such as material are widely used.
In past ten years, researcher is higher and higher to the assembly research interest of nano particle, they are in nanometer
One-dimensional, two-dimentional, the three-dimensional self assembly of structural unit and guide assembling aspect have done a large amount of work.Template is to prepare to receive
The most popular method of rice assembly, achieves fast development, but nano structured unit assembly conduct in ten Nian Liyi of past
The new technology of design of material and preparation, it is necessary to it can accomplish scale production under current processing technology and appointed condition, and
This is exactly the difficult point that current template method prepares Nanoscale assemblies.Therefore, it also needs to simplify assembling flow path, using cheap and easy to get
Mould material develops the magnanimity technology of preparing of Nanoscale assemblies, the final practical application for realizing Nanoscale assemblies.
A series of work has been done in this respect by Yu Shuhong seminar, China Science & Technology University.The seminar is with cheap easy
The business sponge obtained is prepared for a series of unit assembly of nanostructures using sponge as template.They prepare by template of sponge
Gold/cerium dioxide nano line three-dimensional material (with sponge be carrier loaded gold/cerium dioxide nano line three-dimensional material preparation and
Its in-situ reducing p-nitrophenol (English) [J] Science Bulletin in continuous-flow system, 2016,61 (09):
700-705)；Using sponge as macroscopic three dimensional framework template, by simple nano pulp dip-coating means, make silver nanowires
(AgNWs) under the guide of sponge framework template, the AgNWs three-dimensional macro assembly with dual-network structure is formed；Using
Nano pulp dipping process guides the three-dimensional of graphene oxide (GO) to assemble by template of commercial polymer sponge, and preparation is provided
There is the three-dimensional GO macroscopic view assembly of micron order intercommunication hole configurations, corresponding reduced graphene (RGO) can be obtained after HI acid reduction
Three-dimensional macro assembly；Using commercial polymer sponge as template, by nano pulp dipping process, by hydrophobic silica nanometer
Particle (SiO2NPs it) is coated on the skeleton surface of sponge, prepares with the mixture of dimethyl silicone polymer (PDMS) rubber
Porous hydrophobic lipophile material.(the macroscopical Nanoscale assemblies preparation guided based on sponge template and section, application study [D] China
Technology university, 2016).
Shanghai University Lee generation generation uses polyurethane (PU) sponge as basis material, carries out dip-coating by graphene and is modified,
Prepare the polyurethane sponge oil absorption material of super-hydrophobic super-oleophylic；In order to improve graphene in the stability of sponge surface, silicon is utilized
Alkane coupling agent kh-570 is modified graphene, then is loaded to modified graphene on sponge by dip-coating method, thus
Sponge (preparation of oleophilic drainage type sponge and film base water-oil separating material and its performance study [D] loaded to modified graphene
Shanghai University, 2016).
The inspiration of Hunan Normal University Yang Xiao days by seashells bio-adhesive albumen, utilizes dopamine under alkaline environment
Auto polymerization property, it is further using glucose reduction silver ion in polyurethane sponge surface aggregate activity poly-dopamine thin layer
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 super hydrophobic surface (dimethyl silicone polymer/micro-nano silver/poly-dopamine modification of the contact angle greater than 150 °
The preparation and application [J] applied chemistry of super-hydrophobic sponge, 2015,32 (06): 726-732).North China Electric Power University's Zhai's Wenhua is ground
Having studied carefully load has the general sponge of nano silver particles to Hg in water2+The characterization of adsorption of ion has investigated adsorption conditions, finds nanometer
Silver-colored sponge has good removal effect to mercury, and saturated adsorption capacity is up to 2.87mg.g-1(novel nanocomposite materials absorption enrichment
Research [D] the North China Electric Power University of mercury species, 2014).
In addition, assembling Fe there are also using sponge as matrix3O4Particle, molybdenum disulfide, carbon nanotube, titanium dioxide, zinc oxide
Etc. nano materials document report (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 characterization [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 journal (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 University, 2016；Chinese invention patent CN201510443105.9 polyurethane sponge load silver
Graphene titanium dioxide nano-particle composite material, preparation method and application；Chinese invention patent CN201410170974.4 structure
Make the sponge material and preparation method thereof of zinc oxide fine structure modified polyurethane sponge surface；Research of Environmental Sciences, 2016,29
(07):1083-1088；A kind of expanded graphite 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 load has 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 nano material is realized in dip-coating/dipping means, it is this from
Assemble method has randomness and uncontrollability.
Summary of the invention
In view of the above problems, the present invention provides a kind of graphene/nano silver nanocomposites based on sponge template.
The technical scheme is that: (1) after cleaning sponge, it is cut into square, is immersed in quality
In the sodium dodecyl benzene sulfonate aqueous solution of score 1% for 24 hours, bath raio 1:50, vacuum drying after taking-up；(2) prepare 1-100g/L's
Silver nitrate solution is then slowly added into the PAMAM aqueous solution of 1-100g/L, after ultrasonic mixing is uniform, 80-90 DEG C of reaction 1-12h,
Cleaned, be centrifuged repeatedly with ethyl alcohol and deionized water, be dried after obtain nano-Ag particles；(3) by the nano silver in step 2
Particle formulation at 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 use deionized water repeated flushing, drying after taking-up；By above-mentioned sponge impregnating in 1-20g/L graphite oxide
30-60min in aqueous solution, bath raio 1:10 use deionized water repeated flushing, drying, so far by one layer of oxidation stone after taking-up
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 restored, wash, filter, be dried in vacuo after obtain using sponge as mould
The graphene/nano silver composite material of plate.
Preferably, the reducing agent is that hydrazine hydrate, sodium borohydride, sodium citrate, vitamin C, hydroiodic acid, tea are more
One of phenol is a variety of.
Compared with the prior art, the advantages of the present invention are as follows: nano silver and graphene are guided using business sponge as template
Three-dimensional macro self assembly, using 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.
Specific embodiment
The invention will be further elucidated with reference to specific embodiments.
Embodiment 1
(1) after cleaning sponge, it is cut into square, is immersed in the sodium dodecyl benzene sulfonate aqueous solution of mass fraction 1%
For 24 hours, bath raio 1:50, vacuum drying after taking-up；(2) silver nitrate solution for preparing 1g/L, is then slowly added into the PAMAM water of 1g/L
Solution, after ultrasonic mixing is uniform, 80 DEG C of reaction 1h, cleaned, be centrifuged repeatedly with ethyl alcohol and deionized water, be dried after received
Rice Argent grain；(3) nano-Ag particles in step 2 are configured to the aqueous solution of mass fraction 0.1%, it then will be in step 1
Sponge impregnating 30min in nano-silver water solution, bath raio 1:10 use deionized water repeated flushing, drying after taking-up；By above-mentioned sea
Silk floss is immersed in 30min in 1g/L graphene oxide water solution, bath raio 1:10, and deionized water repeated flushing is used after taking-up, dries, so
90 DEG C of reductase 12 h in hydrazine hydrate solution are placed on, washing filters, obtains the graphene/nano using sponge as template after vacuum drying
Rice silver composite material.
Embodiment 2
(1) after cleaning sponge, it is cut into square, is immersed in the sodium dodecyl benzene sulfonate aqueous solution of mass fraction 1%
For 24 hours, bath raio 1:50, vacuum drying after taking-up；(2) silver nitrate solution for preparing 10g/L, is then slowly added into the PAMAM of 10g/L
Aqueous solution, after ultrasonic mixing is uniform, 90 DEG C of reaction 6h, cleaned, be centrifuged repeatedly with ethyl alcohol and deionized water, be dried after obtain
Nano-Ag particles；(3) nano-Ag particles in step 2 are configured to the aqueous solution of mass fraction 1%, it then will be in step 1
Sponge impregnating 60min in nano-silver water solution, bath raio 1:10 use deionized water repeated flushing, drying after taking-up；By above-mentioned sea
Silk floss is immersed in 60min in 10g/L graphene oxide water solution, bath raio 1:10, and deionized water repeated flushing is used after taking-up, dries,
One layer of graphene oxide/nano silver is so far assembled into the surface of sponge, aforesaid operations is then repeated twice, is subsequently placed in lemon
90 DEG C of reduction 12h in lemon acid sodium, washing filter, obtain the graphene/nano silver composite wood using sponge as template after vacuum drying
Material.
Embodiment 3
(1) after cleaning sponge, it is cut into square, is immersed in the sodium dodecyl benzene sulfonate aqueous solution of mass fraction 1%
For 24 hours, bath raio 1:50, vacuum drying after taking-up；(2) silver nitrate solution for preparing 50g/L, is then slowly added into the PAMAM of 50g/L
Aqueous solution, after ultrasonic mixing is uniform, 90 DEG C of reaction 12h, after being cleaned repeatedly with ethyl alcohol and deionized water, be centrifuged, be dried
To nano-Ag particles；(3) nano-Ag particles in step 2 are configured to the aqueous solution of mass fraction 5%, it then will be in step 1
Sponge impregnating in nano-silver water solution 60min, bath raio 1:10, after taking-up use deionized water repeated flushing, drying；It will be above-mentioned
The sponge impregnating 60min in 20g/L graphene oxide water solution, bath raio 1:10 use deionized water repeated flushing after taking-up, dry
It is dry, one layer of graphene oxide/nano silver is so far assembled into the surface of sponge, aforesaid operations is then repeated four times, then sets
60 DEG C of reduction 5h in sodium borohydride, washing filter, obtain answering by the graphene/nano silver of template of sponge after vacuum drying
Condensation material.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.Here all embodiments can not be exhaustive.It is all to belong to this hair
Bright technical solution changes and variations that derived from are still in the scope of protection of the present invention.
Claims (1)
1. the preparation method of the graphene/nano silver nanocomposite based on sponge template, it is characterised in that:
(1) after cleaning sponge, it is cut into square, is immersed in the sodium dodecyl benzene sulfonate aqueous solution of mass fraction 1% for 24 hours,
Bath raio 1:50, vacuum drying after taking-up；(2) silver nitrate solution for preparing 1-100g/L, is then slowly added into 1-100g/L's
PAMAM aqueous solution, after ultrasonic mixing is uniform, 80-90 DEG C of reaction 1-12h is cleaned repeatedly with ethyl alcohol and deionized water, is centrifuged, is dry
Nano-Ag particles are obtained after dry processing；(3) nano-Ag particles in step 2 are configured to the aqueous solution of mass fraction 0.1-5%,
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 solution 30-60min, bath raio 1:10, after taking-up
With deionized water repeated flushing, one layer of graphene oxide/nano silver is so far assembled into the surface of sponge by drying, then weight
Multiple aforesaid operations determine sponge surface graphene oxide/nano silver assembling number of plies as needed；Finally be placed in reducing agent into
Row reduction, the reducing agent are one of hydrazine hydrate, sodium borohydride, sodium citrate, vitamin C, hydroiodic acid, tea polyphenols or more
Kind, washing filters, obtains the graphene/nano silver composite material using sponge as template after vacuum drying.
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| CN109402839B (en) * | 2018-11-18 | 2020-12-11 | 南通源佑纺织科技有限公司 | Antibacterial polyester fiber lining cloth and production process thereof |
| 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 |
| 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 |
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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 |