CN115321488B - Method for preparing self-dispersion nano metal oxide - Google Patents
Method for preparing self-dispersion nano metal oxide Download PDFInfo
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- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 22
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000006185 dispersion Substances 0.000 title abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 31
- 239000002184 metal Substances 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 12
- -1 salt compound Chemical class 0.000 claims abstract description 11
- 239000004094 surface-active agent Substances 0.000 claims abstract description 7
- 150000003839 salts Chemical class 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims abstract description 5
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- 239000007810 chemical reaction solvent Substances 0.000 claims description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 230000003301 hydrolyzing effect Effects 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 claims description 3
- 229920002674 hyaluronan Polymers 0.000 claims description 3
- 229960003160 hyaluronic acid Drugs 0.000 claims description 3
- 229920002401 polyacrylamide Polymers 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 2
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 150000001408 amides Chemical class 0.000 claims description 2
- 150000007942 carboxylates Chemical class 0.000 claims description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 2
- 229920001184 polypeptide Polymers 0.000 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- 102000004196 processed proteins & peptides Human genes 0.000 claims description 2
- 108090000765 processed proteins & peptides Proteins 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 12
- 238000005054 agglomeration Methods 0.000 abstract description 7
- 230000002776 aggregation Effects 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 229910000000 metal hydroxide Inorganic materials 0.000 abstract description 3
- 150000004692 metal hydroxides Chemical class 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 230000007062 hydrolysis Effects 0.000 abstract 1
- 238000006460 hydrolysis reaction Methods 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 8
- 238000003756 stirring Methods 0.000 description 5
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 4
- 239000005751 Copper oxide Substances 0.000 description 4
- 229910000431 copper oxide Inorganic materials 0.000 description 4
- 239000011787 zinc oxide Substances 0.000 description 4
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical compound [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 4
- 238000009826 distribution Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000593 microemulsion method Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000003921 particle size analysis Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- RGHNJXZEOKUKBD-SQOUGZDYSA-M D-gluconate Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O RGHNJXZEOKUKBD-SQOUGZDYSA-M 0.000 description 1
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- NWFNSTOSIVLCJA-UHFFFAOYSA-L copper;diacetate;hydrate Chemical compound O.[Cu+2].CC([O-])=O.CC([O-])=O NWFNSTOSIVLCJA-UHFFFAOYSA-L 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229940050410 gluconate Drugs 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- OXAGUGIXGVHDGD-UHFFFAOYSA-H trizinc;2-hydroxypropane-1,2,3-tricarboxylate;dihydrate Chemical compound O.O.[Zn+2].[Zn+2].[Zn+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O OXAGUGIXGVHDGD-UHFFFAOYSA-H 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/32—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process
- C01B13/328—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process by processes making use of emulsions, e.g. the kerosine process
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Colloid Chemistry (AREA)
- Oxygen, Ozone, And Oxides In General (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a method for preparing self-dispersing nano metal oxide. Adding a weak acid metal salt compound into a solvent system comprising an organic alcohol solvent and a surfactant, heating a precursor which is prepared to obtain the weak acid metal salt compound in an undissolved state in a microwave or high-pressure reaction kettle, realizing slow hydrolysis of metal salt, releasing weak acid at the same time, and uniformly generating metal oxide to obtain the self-dispersible nano metal oxide. The invention utilizes weak acid self-release of weak acid salt to relieve agglomeration of metal hydroxide sol, solves the thermodynamic stability problem of nano material in thermodynamic equilibrium state and agglomeration layering problem brought by interface energy, thereby preparing nano metal oxide with uniform size and shape without secondary dispersion in one step. The technical scheme of the invention has the advantages of simple and quick preparation process, high yield, no need of dispersion, convenient use and the like, and is beneficial to industrial production and application.
Description
Technical Field
The invention relates to a method for preparing self-dispersion nano metal oxide by weak acid self-release, belonging to the technical field of material preparation and application.
Background
The nano metal oxide as one kind of functional material has unique microstructure and several special performances and is significant in industrial and civil application. At present, the preparation method of the small-size metal oxide comprises a solid-phase reaction method, a liquid-phase method, a hydrothermal method, a microemulsion method and a sol-gel method. However, these methods are relatively complex, and the synthesized oxides are difficult to disperse, which affects the application. Before the present invention is made, the literature reports a preparation method of copper oxide nano particles (j. Chemical intermediate, stage 09 in 2010), and proposes some preparation methods of small-size copper oxide, such as a solid-phase reaction method, a liquid-phase method, a hydrothermal method, a microemulsion method, a sol-gel method, etc., wherein the preparation method is carried out by filtering, calcining and drying, and dispersing before use. Therefore, finding a preparation method suitable for self-dispersing metal oxide has important significance for application expansion of nano metal oxide.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides the method for preparing the nano metal oxide, which has the advantages of green, environment-friendly, simple and efficient production process, uniform product size and low cost, by utilizing weak acid self-release.
The technical scheme for realizing the aim of the invention is to provide a method for preparing self-dispersion nano metal oxide, which comprises the following steps:
(1) Adding a weak acid metal salt compound into a reaction solvent system at room temperature to prepare a precursor of which the weak acid metal salt compound is in an undissolved state; the reaction solvent system comprises an organic alcohol solvent and a surfactant;
(2) And (3) putting the precursor prepared in the step (1) into a reaction kettle within 5 minutes, quickly heating the temperature in the reaction kettle to 150-200 ℃ within 30 minutes, starting a built-in stirrer of the reaction kettle, slowly hydrolyzing the weak acid metal salt under the heat preservation condition, releasing the weak acid, and uniformly generating self-dispersed nano metal oxide under the action of the weak acid.
In the technical scheme of the invention, the weak acid metal salt compound comprises one of carboxylate, carbonate, citrate and gluconate. The organic alcohol solvent comprises one of glycol, n-butanol, glycerol, polyethylene glycol and polypropylene glycol. The surfactant comprises one of polyvinylpyrrolidone, polyvinyl amide, polyacrylamide, melamine, organic silicon resin, polypeptide and hyaluronic acid. The molar concentration of the weak acid metal salt compound in the reaction solvent system is 0.01-0.5 mol/L. In the reaction solvent system, the mass percentage of the surfactant is 0.05-0.15%.
In the technical scheme of the invention, the rapid heating method in the step (2) is microwave heating or high-pressure reaction kettle heating; the reaction time is 15-120 min.
The invention is based on the principle that: the weak acid self-release of weak acid salt is utilized to relieve the agglomeration of metal hydroxide sol, and the thermodynamic stability problem in a thermodynamic equilibrium state and the agglomeration layering problem brought by interface energy are solved, so that the nano metal oxide with small size, uniform morphology and no need of secondary dispersion is prepared in one step. Particularly, the weak acid metal salt compound does not need to be dissolved in advance, but reacts while being dissolved in the heating reaction process so as to achieve the synchronism of sol dissolution; the slowly separated weak acid can effectively control sol agglomeration; in order to promote the reaction, stirring is assisted in the reaction process, so that reactants are heated uniformly, and the preparation period is shortened greatly.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention utilizes weak acid self-release of weak acid salt to relieve agglomeration of metal hydroxide sol, overcomes the problems of harsh preparation conditions, long reaction time, difficult dispersion and the like of nano metal oxide, which are unfavorable for wide application, and realizes the one-step preparation of nano metal oxide with uniform size, uniform morphology and no need of secondary dispersion.
2. The novel environment-friendly, low-cost, simple and efficient preparation method provided by the invention has the advantages of simple and rapid preparation process, low energy consumption, high yield, no need of dispersion, convenience in use and the like, and is beneficial to industrial production and application.
Drawings
FIG. 1 is an SEM image of the product prepared in example 1 of the present invention;
FIG. 2 is a TEM electron micrograph of the product prepared in example 1 of the present invention;
FIG. 3 is a graph showing the particle size distribution of nano zinc oxide prepared in example 1 of the present invention.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The technical scheme of the invention is further described below with reference to the attached drawings and specific embodiments.
Example 1
Weighing 100 mL polyethylene glycol, pouring the polyethylene glycol into a beaker, adding a small amount of PVP (polyvinyl pyrrolidone) according to the mass percentage of 0.1%, stirring to form a clear solvent system, pouring the solvent system into a three-neck flask, adding zinc acetate dihydrate according to the concentration of 0.05 mol/L, rapidly heating the three-neck flask to 150 ℃ within 30 minutes under the condition that microwaves are 800W in 5 minutes, starting a stirrer, slowly hydrolyzing the zinc acetate dihydrate under the heat preservation condition, simultaneously releasing weak acid, uniformly generating nano zinc oxide under the action of the weak acid, taking out after 30 minutes, and obtaining the milky nano zinc oxide emulsion.
Referring to fig. 1, an SEM scanning electron microscope image of the nano zinc oxide emulsion prepared according to the technical scheme of the embodiment is shown; as can be seen from FIG. 1, the nano zinc oxide has a rod shape, is uniformly dispersed without agglomeration, has a transverse diameter of about 20nm, and has a longitudinal length of about 100nm.
Referring to fig. 2, a TEM transmission electron microscope image of the nano zinc oxide emulsion prepared in this example is shown.
Referring to fig. 3, a graph of particle size analysis of the nano zinc oxide prepared in this example is shown. The particle size analysis result shows that the average particle size is 80nm, the distribution is uniform, and the self-dispersibility of the nano material is further verified by only one peak.
Example 2
Measuring 100 mL glycol, pouring the glycol into a beaker, adding a small amount of polyacrylamide according to the mass percentage of 0.1%, stirring to form a clear solution as a solvent system, pouring the solvent system into a three-neck flask, adding copper powder acetate monohydrate according to the concentration ratio of 0.05 mol/L, placing the three-neck flask into a high-temperature high-pressure reaction kettle within 5 minutes, quickly heating to 170 ℃ within 30 minutes, starting a stirrer, preserving heat for 60 minutes, slowly hydrolyzing the copper acetate monohydrate, releasing weak acid, and uniformly generating nano copper oxide under the action of the weak acid to obtain brown nano copper oxide emulsion.
Example 3
Weighing 100 mL glycerol, pouring the glycerol into a beaker, adding a small amount of hyaluronic acid according to the mass percentage of 0.15%, and stirring to form a clear solution serving as a solvent system; pouring the solvent system into a three-necked flask, adding zinc citrate dihydrate powder according to the concentration ratio of 0.05 mol/L, placing the three-necked flask into the microwave condition of 800W within 5 minutes, quickly heating to 150 ℃ within 10 minutes, starting stirring, continuously preserving heat for 30 minutes, and taking out to obtain the milky nano zinc oxide emulsion.
Claims (4)
1. A method for preparing self-dispersing nano metal oxide, characterized by comprising the steps of:
(1) Adding a weak acid metal salt compound into a reaction solvent system at room temperature to prepare a precursor of which the weak acid metal salt compound is in an undissolved state; the reaction solvent system consists of an organic alcohol solvent and a surfactant; the weak acid metal salt compound comprises one of carboxylate and citrate; the molar concentration of the weak acid metal salt compound in the reaction solvent system is 0.01-0.5 mol/L; the organic alcohol solvent comprises one of glycol, n-butanol, glycerol, polyethylene glycol and polypropylene glycol;
(2) And (3) putting the precursor prepared in the step (1) into a reaction kettle within 5 minutes, quickly heating the temperature in the reaction kettle to 150-200 ℃ within 30 minutes, starting a built-in stirrer of the reaction kettle, slowly hydrolyzing the weak acid metal salt under the heat preservation condition, releasing the weak acid, and uniformly generating self-dispersed nano metal oxide under the action of the weak acid.
2. A method of preparing self-dispersing nano metal oxides according to claim 1, characterized in that: in the reaction solvent system, the mass percentage of the surfactant is 0.05-0.15%.
3. A method of preparing self-dispersing nano metal oxides according to claim 1, characterized in that: the surfactant comprises one of polyvinylpyrrolidone, polyvinyl amide, polyacrylamide, melamine, organic silicon resin, polypeptide and hyaluronic acid.
4. A method of preparing self-dispersing nano metal oxides according to claim 1, characterized in that: the rapid heating method in the step (2) is microwave heating or high-pressure reaction kettle heating; the reaction time is 15-120 min.
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