CN107556521B - Three-dimensional porous sponge composite material loaded with nano zinc oxide - Google Patents
Three-dimensional porous sponge composite material loaded with nano zinc oxide Download PDFInfo
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- CN107556521B CN107556521B CN201710836746.XA CN201710836746A CN107556521B CN 107556521 B CN107556521 B CN 107556521B CN 201710836746 A CN201710836746 A CN 201710836746A CN 107556521 B CN107556521 B CN 107556521B
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Abstract
The invention discloses a three-dimensional porous sponge composite material loaded with nano zinc oxide, which takes sponge as a carrier and self-assembles nano zinc oxide particles layer by layer through electrostatic action. The invention takes commercial sponge as a template to guide the three-dimensional macroscopic self-assembly of nano zinc oxide, and prepares a three-dimensional macroscopic nano structural unit assembly which has wide application prospect in the fields of adsorption materials, photocatalysis materials, photoelectric devices and biological medicines.
Description
Technical Field
The invention relates to a three-dimensional porous sponge composite material loaded with nano zinc oxide, belonging to the field of nano composite materials.
Background
The inorganic nano material is a material with the size of 1-100nm, has the advantages of simple preparation, low cost, uniform particle size and the like compared with other nano materials, and has wide research and application in the fields of photocatalysis, solar cells, biology, medicine, textile, printing and dyeing, wearable electronic equipment and the like. Among the numerous types of inorganic nanomaterials, zinc oxide occupies an important position. The nano zinc oxide is an important photoelectric semiconductor material, and has a wider forbidden band width (3.37 eV) and a larger exciton confinement energy at room temperature. The nano zinc oxide has a plurality of excellent physical and chemical properties, such as higher chemical stability, no toxicity and non-migration, low dielectric constant, photocatalytic property, fluorescence, piezoelectricity, ultraviolet absorption and scattering capacity and the like, so the nano zinc oxide has important research significance in a plurality of fields and shows attractive application prospects. In recent years, nano zinc oxide has been widely used in the fields of catalysts, gas sensors, semiconductor devices, piezoresistors, piezoelectric devices, field emission displays, ultraviolet light-shielding materials, and the like.
Over the past decade, researchers have become more and more interested in nanoparticle assemblies, which have done a great deal of work in the one-dimensional, two-dimensional, three-dimensional self-assembly of nanostructure elements and directed assembly. The template method is the most common method for preparing nano-assembly, which has been rapidly developed in the past decade, but the nano-structure unit assembly, as a new technology for material design and preparation, must be capable of realizing large-scale production under the current processing technology and equipment conditions, which is a difficulty in preparing nano-assembly by the current template method. Therefore, it is necessary to simplify the assembly process, develop a macro-preparation technique of the nano-assembly by using a template material which is cheap and easily available, and finally realize the practical application of the nano-assembly.
The Shushu Shu hong subject group at the university of science and technology of China does a series of works in this respect. The subject group prepares a series of nanostructured unit assemblies using commercial sponges that are inexpensive and readily available, using sponges as templates. The gold/cerium dioxide nanowire three-dimensional material is prepared by taking sponge as a template (the preparation of the gold/cerium dioxide nanowire three-dimensional material loaded by taking sponge as a carrier and the in-situ reduction of p-nitrophenol (English) in a continuous flow system thereof [ J)]Science Bulletin,2016,61(09): 700-; the method uses sponge as a macroscopic three-dimensional frame template, and silver nanowires (AgNWs) are dipped and coated on the sponge frame template by a simple nano slurryUnder the guidance of (1), forming an AgNWs three-dimensional macroscopic assembly with a double-network structure; adopting a nano slurry dip-coating process, using commercial polymer sponge as a template to guide the three-dimensional assembly of Graphene Oxide (GO), preparing a three-dimensional GO macroscopic assembly with a micron-sized intercommunicated pore structure, and reducing by HI acid to obtain a corresponding Reduced Graphene (RGO) three-dimensional macroscopic assembly; hydrophobic silica nanoparticles (SiO) were impregnated by a nanopaste impregnation process using commercial polymer sponges as templates2NPs) and Polydimethylsiloxane (PDMS) rubber are coated on the surface of the skeleton of the sponge to prepare the porous hydrophobic lipophilic material. (macroscopic nano-assembly preparation and application research based on sponge template guidance [ D)]2016, university of science and technology in china). Polyurethane (PU) sponge is used as a matrix material by Li lifetime of Shanghai university, and is subjected to dip-coating modification by graphene to prepare a super-hydrophobic super-oleophilic polyurethane sponge oil absorption material; in order to improve the stability of graphene on the surface of sponge, graphene is modified by using a silane coupling agent KH-570, and the modified graphene is loaded on the sponge by a dip coating method, so that the modified graphene-loaded sponge (preparation of oleophilic hydrophobic sponge and membrane-based oil-water separation material and performance study thereof [ D ]]University at shanghai, 2016). In addition, the sponge is used as a matrix for assembling nano silver and Fe3O4Literature reports of nano materials such as particles, molybdenum disulfide, carbon nanotubes and titanium dioxide (preparation and application of polydimethylsiloxane/micro-nano silver/polydopamine modified super-hydrophobic sponge [ J)]Application chemistry, 2015,32(06): 726-732; preparation and performance study of oleophylic and hydrophobic sponge and membrane-based oil-water separation Material [ D]University of shanghai, 2016; preparation of super-hydrophobic Polyurethane (PU) sponge and research on oil-water separation characteristics [ D]Harabine university of industry, 2014; preparation and characterization of superhydrophobic sponge based on diazonium chemistry [ D]The university of harbourine industries, 2016; 134 and 138 in the manual lens study, 2017,46 (01); preparation of magnetic response polyurethane sponge and oil absorption performance research [ J]New chemical material, 2017,45(02):239-]The university of river and sea newspaper (Nature science edition), 2017,45(02): 116-; preparation of super-hydrophobic super-oleophylic material and research on oil-water separation performance thereof [ D]Northeast petroleum university, 2016; preparation of super-infiltrating oil-water separation material and performance research thereof [ D]Jiangsu university, 2016; the invention discloses a Chinese patent CN201510443105.9 polyurethane sponge silver-loaded graphene titanium dioxide nanoparticle composite material, a preparation method and application thereof; the Chinese invention patent CN201410170974.4 discloses a sponge material with a zinc oxide fine structure modified polyurethane sponge surface and a preparation method thereof).
Specifically, zinc oxide, Shanghai university Lichen, utilizes micro-nano zinc oxide and palmitic acid to modify and prepare ZnO-PA modified polyurethane sponge with super-hydrophobic and super-lipophilic properties (preparation of lipophilic and hydrophobic sponge and membrane-based oil-water separation material and performance research [ D ]. Shanghai university, 2016). The Beijing university of chemical engineering college of chemical industry uses expanded graphite and zinc oxide as raw materials, adopts a composite modification method to modify polyurethane sponge, and prepares modified polyurethane sponge after the surface of the polyurethane sponge is modified by alcoholic solution of lauric acid under the action of silane coupling agent (environmental science research, 2016,29(07): 1083-1088; China invention patent CN201510470765.6 a polyurethane sponge compositely modified by expanded graphite and zinc oxide and a preparation method thereof). The Chinese invention patent CN201410474510.2 discloses a polyurethane sponge loaded with a hybrid graphene coating and a preparation method thereof, wherein the polyurethane sponge is loaded with a micron zinc oxide hybrid graphene coating, and the mass ratio of zinc oxide to graphene is 5%. However, the above documents mainly rely on dip coating/impregnation means to realize self-assembly of nano zinc oxide, and the self-assembly method has randomness and uncontrollable property.
Disclosure of Invention
Aiming at the defects, the invention provides a three-dimensional porous sponge composite material loaded with nano zinc oxide.
The invention is realized by the following technical scheme: (1) cleaning sponge, cutting into square blocks, soaking in 1% cationic compound water solution at a bath ratio of 1:50 for 24h, taking out, and vacuum drying; (2) preparing 1mol/L zinc chloride solution, dropwise adding 1mol/L sodium hydroxide aqueous solution, ultrasonically mixing the sodium hydroxide solution and the zinc chloride solution uniformly, slowly adding sodium dodecyl sulfate, ultrasonically mixing the sodium dodecyl sulfate and the zinc chloride solution for 2 hours, transferring the mixture into a reaction kettle at the temperature of 160 ℃, reacting for 6-12 hours, repeatedly cleaning with ethanol and deionized water, centrifuging, and drying to obtain zinc oxide nanoparticles; (3) respectively preparing 1-100g/L and 1mol/L aqueous solutions of PAMAM and zinc nitrate hexahydrate, wherein the volume ratio of the PAMAM to the zinc nitrate hexahydrate aqueous solution is 1:1-5:1, uniformly mixing and stirring, transferring the mixture into a reaction kettle, reacting for 5 hours at 200 ℃, repeatedly washing with ethanol and deionized water, centrifuging and drying to obtain zinc oxide nanoparticles; (4) preparing the zinc oxide nano particles in the step two into an aqueous solution with the mass fraction of 0.1-5%, then soaking the sponge in the aqueous solution of the nano zinc oxide for 30-60min at a bath ratio of 1:10, taking out, repeatedly washing with deionized water, and drying; preparing the zinc oxide nano particles in the third step into an aqueous solution with the mass fraction of 0.1-5%, soaking the sponge in the aqueous solution of the nano zinc oxide for 30-60min at a bath ratio of 1:10, taking out, repeatedly washing with deionized water, drying, assembling a layer of nano zinc oxide particles on the surface of the sponge, repeating the operation, and determining the number of layers of the nano zinc oxide particles on the surface of the sponge according to the needs.
Preferably, the cationic compound is one or more of amino-terminated hyperbranched polymer, PAMAM, chitosan, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, polydopamine, 2, 3-epoxypropyltrimethylammonium chloride, octyldodecyldimethylammonium chloride and polyethyleneimine.
Compared with the prior art, the invention has the advantages that: the three-dimensional macroscopic self-assembly of the nano zinc oxide is guided by using commercial sponge as a template, and the electrostatic action among the nano zinc oxide is used as a film forming driving force to prepare the three-dimensional macroscopic structure unit assembly which has wide application prospect in the fields of adsorption materials, photocatalysis materials, photoelectric devices and biomedicine.
Detailed Description
The invention will be further illustrated with reference to specific embodiments.
Example 1
(1) Cleaning sponge, cutting into square blocks, soaking in 1% by mass of amino-terminated hyperbranched polymer aqueous solution for 24h at a bath ratio of 1:50, taking out, and vacuum drying; (2) preparing 1mol/L zinc chloride solution, dropwise adding 1mol/L sodium hydroxide aqueous solution, wherein the volume ratio of the sodium hydroxide solution to the zinc chloride solution is 1:2, ultrasonically mixing uniformly, slowly adding sodium dodecyl sulfate, wherein the mass ratio of the sodium dodecyl sulfate to the zinc chloride is 1:1, ultrasonically reacting for 2 hours, moving the mixture into a reaction kettle at 160 ℃ for 6 hours, and repeatedly cleaning, centrifuging and drying the mixture by using ethanol and deionized water to obtain zinc oxide nanoparticles; (3) respectively preparing 1g/L and 1mol/L aqueous solutions of PAMAM and zinc nitrate hexahydrate, wherein the volume ratio of the PAMAM to the zinc nitrate hexahydrate aqueous solution is 1:1, uniformly mixing and stirring, moving the mixture into a reaction kettle for reaction at 200 ℃ for 5 hours, and repeatedly washing, centrifuging and drying the mixture by using ethanol and deionized water to obtain zinc oxide nano particles; (4) preparing the zinc oxide nano particles in the step two into an aqueous solution with the mass fraction of 0.1%, then soaking the sponge in the aqueous solution of the nano zinc oxide for 30min at the bath ratio of 1:10, taking out, repeatedly washing with deionized water, and drying; preparing the zinc oxide nano particles in the third step into an aqueous solution with the mass fraction of 0.1%, soaking the sponge in the aqueous solution of nano zinc oxide for 30min at a bath ratio of 1:10, taking out, repeatedly washing with deionized water, and drying to obtain the three-dimensional porous sponge composite material loaded with nano zinc oxide.
Example 2
(1) Cleaning sponge, cutting into square blocks, soaking in 1% by mass of polyethyleneimine water solution for 24h at a bath ratio of 1:50, taking out, and vacuum drying; (2) preparing 1mol/L zinc chloride solution, dropwise adding 1mol/L sodium hydroxide aqueous solution, wherein the volume ratio of the sodium hydroxide solution to the zinc chloride solution is 1:1, ultrasonically mixing uniformly, slowly adding sodium dodecyl sulfate, wherein the mass ratio of the sodium dodecyl sulfate to the zinc chloride is 2:1, ultrasonically reacting for 2h, moving the mixture into a reaction kettle at 160 ℃ for 9h, and repeatedly cleaning, centrifuging and drying the mixture by using ethanol and deionized water to obtain zinc oxide nanoparticles; (3) respectively preparing 10g/L and 1mol/L aqueous solutions of PAMAM and zinc nitrate hexahydrate, wherein the volume ratio of the PAMAM to the zinc nitrate hexahydrate is 2:1, uniformly mixing and stirring, moving the mixture into a reaction kettle for reaction at 200 ℃ for 5 hours, and repeatedly washing, centrifuging and drying the mixture by using ethanol and deionized water to obtain zinc oxide nano particles; (4) preparing the zinc oxide nano particles in the step two into an aqueous solution with the mass fraction of 1%, then soaking the sponge in the aqueous solution of nano zinc oxide for 50min at a bath ratio of 1:10, taking out, repeatedly washing with deionized water, and drying; preparing the zinc oxide nano particles in the third step into an aqueous solution with the mass fraction of 1%, soaking the sponge in the aqueous solution of the nano zinc oxide for 50min at a bath ratio of 1:10, taking out the sponge, repeatedly washing the sponge with deionized water, drying the sponge until a layer of nano zinc oxide particles are assembled on the surface of the sponge, and repeating the operation once to obtain the three-dimensional porous sponge composite material loaded with the nano zinc oxide.
Example 3
(1) Cleaning sponge, cutting into square blocks, soaking in 1 wt% 2, 3-epoxypropyl trimethyl ammonium chloride water solution for 24 hr at a bath ratio of 1:50, taking out, and vacuum drying; (2) preparing 1mol/L zinc chloride solution, then dropwise adding 1mol/L sodium hydroxide aqueous solution, wherein the volume ratio of the sodium hydroxide solution to the zinc chloride solution is 2:1, ultrasonically mixing uniformly, slowly adding sodium dodecyl sulfate, wherein the mass ratio of the sodium dodecyl sulfate to the zinc chloride is 3:1, ultrasonically reacting for 2h, moving the mixture into a reaction kettle at 160 ℃ for 12h, and repeatedly cleaning, centrifuging and drying the mixture by using ethanol and deionized water to obtain zinc oxide nanoparticles; (3) respectively preparing 20g/L and 1mol/L aqueous solutions of PAMAM and zinc nitrate hexahydrate, wherein the volume ratio of the PAMAM to the zinc nitrate hexahydrate is 5:1, uniformly mixing and stirring, moving the mixture into a reaction kettle for reaction at 200 ℃ for 5 hours, and repeatedly washing, centrifuging and drying the mixture by using ethanol and deionized water to obtain zinc oxide nano particles; (4) preparing the zinc oxide nano particles in the step two into an aqueous solution with the mass fraction of 5%, then soaking the sponge in the aqueous solution of nano zinc oxide for 60min at a bath ratio of 1:10, taking out, repeatedly washing with deionized water, and drying; preparing the zinc oxide nano particles in the third step into an aqueous solution with the mass fraction of 5%, soaking the sponge in the aqueous solution of the nano zinc oxide for 60min at a bath ratio of 1:10, taking out the sponge, repeatedly washing the sponge with deionized water, drying the sponge until a layer of nano zinc oxide particles are assembled on the surface of the sponge, and repeating the operation twice to obtain the three-dimensional porous sponge composite material loaded with the nano zinc oxide.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. Not all embodiments are exhaustive. All obvious changes and modifications of the present invention are within the scope of the present invention.
Claims (6)
1. The three-dimensional porous sponge composite material loaded with nano zinc oxide is characterized in that: using the sponge pretreated by the cationic compound as a carrier, and carrying out layer-by-layer self-assembly on nano zinc oxide particles through electrostatic action;
the preparation steps are as follows: (1) cleaning sponge, cutting into square blocks, soaking in 1% cationic compound water solution at a bath ratio of 1:50 for 24h, taking out, and vacuum drying; (2) preparing 1mol/L zinc chloride solution, then dropwise adding 1mol/L sodium hydroxide aqueous solution, ultrasonically mixing uniformly, slowly adding sodium dodecyl sulfate, ultrasonically treating for 2 hours, moving to a reaction kettle for reacting for 6-12 hours at 160 ℃, repeatedly cleaning with ethanol and deionized water, centrifuging, and drying to obtain zinc oxide nanoparticles; (3) respectively preparing 1-100g/L and 1mol/L aqueous solutions of PAMAM and zinc nitrate hexahydrate, mixing and stirring uniformly, transferring to a reaction kettle for reaction at 200 ℃ for 5 hours, repeatedly cleaning with ethanol and deionized water, centrifuging, and drying to obtain zinc oxide nanoparticles; (4) preparing the zinc oxide nano particles in the step two into an aqueous solution with the mass fraction of 0.1-5%, then soaking the sponge in the aqueous solution of the nano zinc oxide for 30-60min at a bath ratio of 1:10, taking out, repeatedly washing with deionized water, and drying; preparing the zinc oxide nano particles in the third step into an aqueous solution with the mass fraction of 0.1-5%, soaking the sponge in the aqueous solution of the nano zinc oxide for 30-60min at a bath ratio of 1:10, taking out, repeatedly washing with deionized water, drying, assembling a layer of nano zinc oxide particles on the surface of the sponge, repeating the operation, and determining the number of layers of the nano zinc oxide particles on the surface of the sponge according to the needs.
2. The three-dimensional porous sponge composite material loaded with nano zinc oxide according to claim 1, wherein the cationic compound is one or more of amino-terminated hyperbranched polymer, PAMAM, chitosan, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, polydopamine, 2, 3-epoxypropyltrimethylammonium chloride, octyldodecyldimethylammonium chloride and polyethyleneimine.
3. The three-dimensional porous sponge composite material loaded with nano zinc oxide according to claim 1, characterized in that the volume ratio of the sodium hydroxide solution and the zinc chloride solution is 1:2-2: 1.
4. The three-dimensional porous sponge composite material loaded with nano zinc oxide according to claim 1, wherein the mass ratio of the sodium dodecyl sulfate to the zinc chloride is 1:1-3: 1.
5. The three-dimensional porous sponge composite material loaded with nano zinc oxide according to claim 1, wherein the volume ratio of the PAMAM to the zinc nitrate hexahydrate aqueous solution is 1:1-5: 1.
6. The three-dimensional porous sponge composite material loaded with nano zinc oxide obtained by the preparation method of claim 1.
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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 |
| CN110444730B (en) * | 2019-08-19 | 2021-08-27 | 中南大学 | Preparation method and application of three-dimensional network structure nano-layer zinc cathode |
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