CN113979466A - ZnO@SiO2Preparation method of nano capsule - Google Patents
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
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- C01G9/02—Oxides; Hydroxides
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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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
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Abstract
The invention relates to ZnO @ SiO2A preparation method of nano capsules belongs to the technical field of nano materials, and comprises the following steps: step 1, preparing organic acid zinc salt; step 2, ZnO @ SiO2And (3) preparing the nano composite material. The invention relates to ZnO @ SiO2The preparation method of the nano-capsule comprises the steps of utilizing long-chain carboxylate as a structure directing agent, ethyl orthosilicate and aminosilane as silicon sources, utilizing organic acid zinc salt as a precursor, carrying out a series of continuous spontaneous reactions in a water-alcohol system in sequence to obtain an organic-inorganic hybrid nano-material, and finally calcining to obtain ZnO @ SiO2A nanocapsule; the zinc salt of the organic acid is connected with the long-chain sodium carboxylate serving as a structure guiding agent by utilizing ligand exchange reaction, so that a large amount of metal ions can be introduced into the silicon dioxide matrix; the preparation method has mild reaction conditions, does not need to add an acid or alkaline catalyst, and can obtain the ZnO nanoparticles with better dispersity.
Description
Technical Field
The invention relates to a method for preparing nano capsules, in particular to a method for preparing nano capsulesIt relates to ZnO @ SiO2A preparation method of nano capsules belongs to the technical field of nano materials.
Background
ZnO nanoparticles have excellent optical characteristics, no toxicity, wide raw materials and the like, and are always taken as research hotspots in the field of nano science, but the ZnO nanoparticles are extremely easy to agglomerate to cause serious reduction of functionality, so that the ZnO nanoparticles need to be dispersed in a carrier material to stabilize the performance of the carrier material, and SiO (silicon oxide) in a plurality of carrier materials2Has the advantages of high stability, ultraviolet permeability, easy preparation and the like, and has SiO with large specific surface area2Composite materials as carriers have become hot research points in many fields such as physics, chemistry, materials and life science in recent years, and therefore become ideal carrier materials for a plurality of nanoparticles.
The method for preparing the hollow silica-based nano composite material by the template method is the first choice and the mainstream method at present, but the metal nano particles with better dispersity and considerable loading capacity are difficult to obtain. In addition, strong alkaline substances such as ammonia water and sodium hydroxide are used as catalysts in the method, potential experimental hazards exist, metal nanoparticles are easy to damage, the environment is greatly harmed due to the large amount of the metal nanoparticles, and the synthetic process is complicated. Therefore, there is a need to find a simple way to obtain silica matrix composite capsules containing a large loading.
Disclosure of Invention
The purpose of the invention is: in order to overcome the defects in the prior art, the ZnO @ SiO is provided2The preparation method of the nano capsule has mild reaction conditions, continuous and spontaneous reaction, no need of adding an acid or alkaline catalyst, low complexity of preparation steps and capability of obtaining ZnO nano particles with better dispersibility.
The technical scheme for solving the technical problems is as follows:
ZnO @ SiO2The preparation method of the nano capsule comprises the following steps:
step 1, preparation of organic acid zinc salt: sequentially putting organic carboxylic acid and zinc oxide into 100mL of high-purity water according to a certain proportion, and reacting for 2-24 h in a water bath at 40-90 ℃ to generate organic acid zinc salt serving as a metal particle precursor;
step 2, ZnO @ SiO2Preparing a nano composite material: dissolving long-chain sodium carboxylate in high-purity water, performing ultrasonic treatment and vigorous stirring until the long-chain sodium carboxylate is completely dissolved, dissolving the generated organic acid zinc salt in a mixed solution of water and absolute ethyl alcohol, dropwise adding the organic acid zinc salt into a high-purity water solution containing the long-chain sodium carboxylate, and dropwise adding a mixture of tetraethoxysilane and aminosilane into the solution after uniform dispersion; finally, controlling the stirring speed to be 600r/min, reacting for 12-96 h at normal temperature and pressure, then performing centrifugal separation, drying the obtained solid, then placing the dried solid in a muffle furnace, calcining in air atmosphere, wherein the heating rate is 1-10 ℃/min, the heat preservation temperature is 500-660 ℃, and the heat preservation time is 0.5-4 h, thus obtaining ZnO @ SiO2And (4) nanocapsules.
Furthermore, the long-chain carboxylate is a structure directing agent, the ethyl orthosilicate and the aminosilane are silicon sources, and the zinc salt of the organic acid is a precursor.
Still further, the organic carboxylic acid is an α -halopropionic acid; the molar ratio of the organic carboxylic acid to the zinc oxide is 2-10: 1.
Further, the long-chain sodium carboxylate is a long-chain sodium salt with sixteen or more carbon atoms.
Still further, the aminosilane is an amino-bearing organosilane; the volume ratio of the ethyl orthosilicate to the aminosilane is 1: 2-4 mixing.
Furthermore, the mass concentration of the zinc salt of the organic acid is 0.025 g/mL-0.5 g/mL.
Further, the water and the absolute ethyl alcohol are mixed according to the volume ratio of 1-3: 1 and mixing.
Furthermore, the centrifugal rate in the second step is 4000 r/min-9500 r/min.
The invention has the beneficial effects that: the preparation method comprises the steps of utilizing long-chain carboxylate as a structure directing agent, tetraethoxysilane and aminosilane as silicon sources, utilizing organic acid zinc salt as a precursor, sequentially carrying out a series of continuous spontaneous reactions in a water-alcohol system to obtain an organic-inorganic hybrid nano material, and finally carrying out a series of continuous spontaneous reactions on the organic-inorganic hybrid nano materialObtaining ZnO @ SiO through calcination2A nanocapsule; the zinc salt of the organic acid is connected with the long-chain sodium carboxylate serving as a structure guiding agent by utilizing ligand exchange reaction, so that a large amount of metal ions can be introduced into the silicon dioxide matrix; the preparation method has mild reaction conditions, does not need to add an acid or alkaline catalyst, has low complexity of preparation steps, and can obtain the ZnO nanoparticles with better dispersibility.
Drawings
FIG. 1 shows ZnO @ SiO in the present invention2SEM images of nanocapsules;
FIG. 2 shows ZnO @ SiO in the present invention2TEM pictures of nanocapsules;
FIG. 3 shows ZnO @ SiO in the present invention2XRD pictures of nanocapsules.
Detailed Description
The principles and features of the present invention are described below in conjunction with the accompanying fig. 1-3, which are provided by way of example only to illustrate the present invention and not to limit the scope of the present invention.
Example 1
A preparation method of ZnO @ SiO2 nanocapsules comprises the following steps:
step 1, preparation of zinc alpha-bromopropionate: sequentially putting 0.01mol of zinc oxide and 0.02mol of alpha-bromopropionic acid into a single-neck round-bottom flask filled with 100ml of high-purity water, reacting for 4 hours in a water bath at 60 ℃, filtering to obtain a clear solution, and distilling off the solvent by using a rotary evaporator to obtain a white solid, namely the zinc salt of alpha-bromopropionic acid;
step 2, preparing the ZnO @ SiO2 nanocomposite: dissolving 0.5g of sodium octadecenoate in 18mL of high-purity water, performing ultrasonic treatment until the sodium octadecenoate is completely dispersed, dissolving 0.45g of alpha-bromozinc propionate in 6mL of water and 6mL of absolute ethyl alcohol, dropwise adding the solution into the sodium octadecenoate solution, and uniformly stirring; then adding 0.6mL of ethyl orthosilicate and 1.2mL of 3-aminopropyltriethoxysilane into the solution, controlling the stirring rate to be 600r/min, reacting for 12h at normal temperature and pressure, centrifuging at the rate of 8000r/min, drying the obtained solid, putting the dried solid into a muffle furnace, calcining in the air atmosphere at the temperature rise rate of 1 ℃/min, the heat preservation temperature of 600 ℃, and the heat preservation time of 4h to finally obtain ZnO @ SiO2And (4) nanocapsules.
Example 2
A preparation method of ZnO @ SiO2 nanocapsules comprises the following steps:
step 1, preparation of zinc salt of alpha-chloropropionic acid: putting 0.01mol of zinc oxide and 0.02mol of alpha-chloropropionic acid into a single-neck round-bottom flask filled with 100ml of high-purity water in sequence, reacting for 24 hours in a water bath at 60 ℃, filtering to obtain a clear solution, and evaporating the solvent by using a rotary evaporator to obtain a white solid, namely the zinc salt of alpha-chloropropionic acid;
step 2, ZnO @ SiO2Preparing a nano composite material: dissolving 0.5g of sodium laurate in 18mL of high-purity water, performing ultrasonic treatment until the sodium laurate is completely dispersed, dissolving 0.45g of alpha-zinc chloropropionate in 6mL of water and 6mL of absolute ethyl alcohol, dropwise adding the alpha-zinc chloropropionate into the sodium laurate solution, and uniformly stirring; then adding 0.6mL of ethyl orthosilicate and 1.2mL of 3-aminopropyltriethoxysilane into the solution, controlling the stirring rate to be 600r/min, reacting for 12h at normal temperature and pressure, centrifuging at the rate of 8000r/min, drying the obtained solid, putting the dried solid into a muffle furnace, calcining in the air atmosphere at the temperature rise rate of 1 ℃/min, the heat preservation temperature of 600 ℃, and the heat preservation time of 4h to finally obtain ZnO @ SiO2And (4) nanocapsules.
Two groups of ZnO @ SiO obtained2The nanocapsules were collected and analyzed for any one of the groups of materials, as shown in figures 1, 2 and 3:
(1) it can be seen from FIG. 1 that the resulting material was in a regular spherical shape, the average particle diameter was about 400nm, and an open structure was observed;
(2) as can be seen from fig. 2, the obtained material is a hollow structure, and ZnO nanoparticles are dispersed on the silica wall;
(3) as can be seen from fig. 3, a series of diffraction peaks appear at 31.7 °, 34.6 °, 36.5 °, 47.6 °, 56.5 °, 62.8 °, 68.3 ° and 69.2 °, respectively, corresponding to the (100), (002), (101), (102), (110), (103), (112) and (201) crystal planes of the ZnO nanoparticles, respectively, and as compared with the standard card, the ZnO nanoparticles produced are hexagonal system with unit cell parameters a 3.253 and c 5.209(JCPDS No. 80-0075).
The preparation method of the ZnO @ SiO2 nanocapsule comprises the steps of utilizing long-chain carboxylate as a structure directing agent, ethyl orthosilicate and aminosilane as silicon sources, utilizing organic acid zinc salt as a precursor, carrying out a series of continuous spontaneous reactions in a water-alcohol system in sequence to obtain an organic-inorganic hybrid nanomaterial, and finally calcining to obtain ZnO @ SiO2A nanocapsule; the zinc salt of the organic acid is connected with the long-chain sodium carboxylate serving as a structure guiding agent by utilizing ligand exchange reaction, so that a large amount of metal ions can be introduced into the silicon dioxide matrix; the preparation method has mild reaction conditions, does not need to add an acid or alkaline catalyst, has low complexity of preparation steps, and can obtain the ZnO nanoparticles with better dispersibility.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. ZnO @ SiO2The preparation method of the nano capsule is characterized by comprising the following steps:
step 1, preparation of organic acid zinc salt: sequentially putting organic carboxylic acid and zinc oxide into 100mL of high-purity water according to a certain proportion, and reacting for 2-24 h in a water bath at 40-90 ℃ to generate organic acid zinc salt serving as a metal particle precursor;
step 2, ZnO @ SiO2Preparing a nano composite material: dissolving long-chain sodium carboxylate in high-purity water, performing ultrasonic treatment and vigorous stirring until the long-chain sodium carboxylate is completely dissolved, dissolving the generated organic acid zinc salt in a mixed solution of water and absolute ethyl alcohol, dropwise adding the organic acid zinc salt into a high-purity water solution containing the long-chain sodium carboxylate, and dropwise adding a mixture of tetraethoxysilane and aminosilane into the solution after uniform dispersion; finally, controlling the stirring speed to be 600r/min, reacting for 12-96 h at normal temperature and pressure, then performing centrifugal separation, drying the obtained solid, then placing the dried solid in a muffle furnace, calcining in air atmosphere, wherein the heating rate is 1-10 ℃/min, the heat preservation temperature is 500-660 ℃, and the heat preservation time is 0.5-4 h, thus obtaining ZnO @ SiO2And (4) nanocapsules.
2. The ZnO @ SiO of claim 12The preparation method of the nano capsule is characterized by comprising the following steps: the long-chain carboxylate is a structure directing agent, the ethyl orthosilicate and the aminosilane are silicon sources, and the zinc salt of the organic acid is a precursor.
3. The ZnO @ SiO of claim 12The preparation method of the nano capsule is characterized by comprising the following steps: the organic carboxylic acid is alpha-halopropionic acid; the molar ratio of the organic carboxylic acid to the zinc oxide is 2-10: 1.
4. The ZnO @ SiO of claim 12The preparation method of the nano capsule is characterized by comprising the following steps: the long-chain sodium carboxylate is long-chain sodium salt with more than sixteen carbon atoms.
5. The ZnO @ SiO of claim 12The preparation method of the nano capsule is characterized by comprising the following steps: the aminosilane is organosilane with amino; the volume ratio of the ethyl orthosilicate to the aminosilane is 1: 2-4 mixing.
6. The ZnO @ SiO of claim 12The preparation method of the nano capsule is characterized by comprising the following steps: the mass concentration of the organic acid zinc salt is 0.025 g/mL-0.5 g/mL.
7. The ZnO @ SiO of claim 12The preparation method of the nano capsule is characterized by comprising the following steps: the water and the absolute ethyl alcohol are mixed according to the volume ratio of 1-3: 1 and mixing.
8. The ZnO @ SiO of claim 12The preparation method of the nano capsule is characterized by comprising the following steps: and the centrifugal rate in the second step is 4000 r/min-9500 r/min.
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| CN114921145A (en) * | 2022-06-10 | 2022-08-19 | 洛阳大豫实业有限公司 | Modified graphene anticorrosive paint and preparation method thereof |
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| JP2001038193A (en) * | 1999-07-28 | 2001-02-13 | Nippon Millipore Kk | Production of composite silica microcapsule, and method for controlling immobilization and slow releasing action of core substance of composite silica microcapsule |
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