CN115159563A - Method for preparing amphoteric oxide microspheres in mild manner by using aqueous two-phase system - Google Patents
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Abstract
The invention discloses a method for preparing amphoteric oxide microspheres by a double aqueous phase system in a mild way, which comprises the following steps: adding 2.2-5.5g of ethyl acetate into precursor liquid of amphoteric oxide acid salt-small molecular alcohol at room temperature, stirring to form a two-aqueous-phase system, sealing, standing, and performing two-hydrolysis reaction to generate white precipitate; filtering, washing and drying to obtain the amphoteric oxide microspheres. The invention realizes that the diffusion rate of reaction particles is controlled by the condition of a phase interface through a double aqueous phase system of amphoteric oxide acid salt-micromolecule alcohol, thereby reducing the precipitation rate and obtaining amphoteric oxide microspheres with uniform particle size; the precipitation strategy takes small molecular alcohol, ethyl acetate and other green raw materials to participate in product synthesis, and has simple and convenient operation and low cost; meanwhile, the method has certain universality, and provides a technical idea for preparing amphoteric oxide from alkaline salt solution and expanding a liquid-phase precipitation system to a double water-phase system.
Description
Technical Field
The invention relates to the technical field of amphoteric oxide microspheres, in particular to a method for preparing amphoteric oxide microspheres by a double aqueous phase system in a mild way.
Background
The micro-nano material has wide application in the fields of catalysis, energy conversion, storage and the like, and the control of the morphology and the particle size of the micro-nano material has important significance for the high-efficiency utilization of the material. Among them, the sphere is the most stable morphology in nature. For metal oxides/hydroxides, the microsphere structure generally has the advantages of relatively high mechanical strength, high surface area, easy coating or loading with other metals, and low fluid resistance (low viscosity effect) [ Yash B, meiwen W, jian L, et al. Synthesis and applications of pore non-silicon metal oxide microspheres [ J ]. Chemical Society Reviews,2016,45 (21): 6013-6047]. Therefore, a green and simple strategy for synthesizing micro-nano spherical metal oxide/hydroxide is developed, and the method has important significance for preparing microsphere composite materials and etchable templates with hollow structures related to the micro-nano spherical metal oxide/hydroxide.
However, the traditional liquid phase precipitation method has the problem that the precipitation rate is not easy to control to cause uncontrollable morphology when the micro-nano material is prepared. Generally, the method generally selects raw materials with slow reaction rate to obtain products with controllable morphology, and the essence of the method is to control the precipitation rate by regulating the factors such as ionization degree and supersaturation degree of particles in the system [ Lai W-H, wang Y-X, wang Y, et al. Morphology of organic nanomaterials growth by precipitation method of natural chemistry,2019,11 (8): 695-701 ].
In the national patent network, publication No. CN 110240193A discloses a preparation method of amphoteric metal oxide microspheres, which comprises adding amide precipitant into precursor solution to obtain a series of amphoteric metal oxide microspheres and composite microspheres thereof; the method controls the precipitation rate through slow double hydrolysis reaction to obtain the product with the microsphere shape, has the advantages of low cost, simple process, mass production and the like, but has the defect that the amide substance is a low-toxicity raw material.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a method for preparing amphoteric oxide microspheres mildly by using a two-aqueous-phase system, which has the advantages of taking green raw materials of small molecular alcohol and ethyl acetate to participate in product synthesis, along with simple and convenient operation, low cost and the like, and solves the problem that amide substances in the raw materials have low toxicity.
(II) technical scheme
In order to realize the purposes of taking green raw materials, namely small molecular alcohol and ethyl acetate to participate in product synthesis, simple and convenient operation and low cost, the invention provides the following technical scheme:
a method for preparing amphoteric oxide microspheres in a mild manner by using an aqueous two-phase system comprises the following steps:
s1, adding 2.2-5.5g of ethyl acetate into a precursor liquid of amphoteric oxide acid salt-small molecular alcohol at room temperature, and stirring to form a two-aqueous-phase system;
s2, carrying out double hydrolysis reaction on the double aqueous phase system obtained in the step S1 to generate white precipitate;
s3, filtering the white precipitate obtained in the step S2, and washing with deionized water and absolute ethyl alcohol in sequence;
and S4, drying the washed white precipitate in the step S3 to obtain the amphoteric oxide microspheres.
Preferably, in step S1, the amphoteric oxidate precursor solution is an aqueous solution of sodium stannate, sodium silicate and self-made sodium zincate, and the small molecular alcohol is absolute ethyl alcohol and propanol.
Preferably, in the step S1, the amount of the amphoteric oxysalt is 0.5-1.22g, and H in the aqueous two-phase system 2 The mass of O is 10-30g, and the mass of alcohol is 11.4-26.7g.
Preferably, in the step S2, a sealing operation is required to perform the double hydrolysis reaction.
Preferably, in the step S2, the hydrolysis temperature is 24-26 ℃, and the hydrolysis time is 2h.
Preferably, in the step S2, the double hydrolysis reaction is performed under a standing condition.
Preferably, in the step S4, the prepared SnO 2 The microspheres have an average particle size of 0.2-1 μm.
Preferably, in the step S4, the obtained SiO is prepared 2 The microspheres have an average particle size of 1-2 μm.
Preferably, in the step S4, the average particle size of the prepared ZnO microspheres is 0.4-8 μm.
Preferably, in the step S4, the temperature during drying is set to be 60-62 ℃, and the drying time is 12-15h.
(III) advantageous effects
Compared with the prior art, the method for preparing the amphoteric oxide microspheres by using the aqueous two-phase system provided by the invention has the following beneficial effects:
1. the method for preparing the amphoteric oxide microspheres in the double aqueous phase system mildly takes the green raw materials of micromolecule alcohol and ethyl acetate to participate in product synthesis, is simple and convenient to operate and low in cost, has certain universality, and provides an idea for preparing amphoteric oxides from alkaline salt solutions and expanding a liquid phase precipitation system to the double aqueous phase system.
2. The method for preparing the amphoteric oxide microspheres by the double aqueous phase system mildly develops a general method for preparing amphoteric oxide from alkaline salt solution by matching different precursor solutions and ethyl acetate, has good repeatability, and the synthesized amphoteric oxide materials such as ZnO and the like have good application potential in the fields of gas sensors, batteries, catalysis and the like.
3. According to the method for preparing the amphoteric oxide microspheres in a mild double-aqueous-phase system, the precipitation rate can be controlled by controlling the system interface condition (alcohol dosage) through an auxiliary synthesis strategy of a salt-alcohol double-aqueous-phase system, so that the product morphology is regulated, and the diffusion rate of reaction particles is controlled by the phase interface condition through the double-aqueous-phase system of amphoteric oxide acid salt-small molecular alcohol, so that the precipitation rate is reduced, and the amphoteric oxide microspheres with uniform particle sizes are obtained.
Drawings
FIG. 1 is SEM and TEM images of microspheres prepared in example 1 of the present invention.
FIG. 2 is SEM and TEM images of microspheres prepared in example 2 of the present invention.
FIG. 3 is an SEM and TEM image of microspheres prepared in example 3 of the present invention.
FIG. 4 is SEM and TEM images of microspheres prepared in example 4 of the present invention.
FIG. 5 is SEM and TEM images of microspheres prepared in example 5 of the present invention.
Figure 6 is an XRD pattern of microspheres prepared according to various embodiments of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example (b):
the method for preparing the amphoteric oxide microspheres by the aqueous two-phase system comprises the following steps:
s1, adding 2.2-5.5g of ethyl acetate into a precursor liquid of amphoteric oxide acid salt-small molecular alcohol at room temperature, and stirring to form a two-aqueous-phase system;
s2, carrying out double hydrolysis reaction on the double aqueous phase system obtained in the step S1 to generate white precipitate;
s3, filtering the white precipitate obtained in the step S2, and washing with deionized water and absolute ethyl alcohol in sequence;
and S4, drying the washed white precipitate in the step S3 to obtain the amphoteric oxide microspheres.
In the amphoteric oxide salt adopted in the embodiment of the invention, the sodium zincate solution is self-made in a laboratory, and the preparation process comprises the following steps: at room temperature, 0.81g of crude ZnO powder is added into 12mL of 10M NaOH, dissolved under stirring, and filtered to obtain a uniform clear solution; all other components are commercial products.
Example one
The method for preparing the amphoteric oxide microspheres by the aqueous two-phase system comprises the following specific steps:
0.5g of Na is added at room temperature 2 SnO 3 Added to 20.0g of deionized water, dissolved with stirring, and then 17.0g of n-propanol was added. Stirring vigorously for 1min, and standing for 5min to obtain propanol-sodium stannate aqueous two-phase system; adding 2.2g of ethyl acetate into the obtained solution, sealing and standing for 2h, filtering the obtained white precipitate, washing the white precipitate with deionized water to neutrality, washing the white precipitate with ethanol once, and drying the white precipitate in a forced air drying oven at 60 ℃ for 12h to obtain SnO 2 And (3) microspheres.
As shown in FIG. 1, the resultant SnO 2 The surface of the microsphere is smooth, and the average grain diameter is 0.2-1 mu m.
Example two
The method for preparing the amphoteric oxide microspheres by the aqueous two-phase system is basically the same as that in the example 1, and the difference is that the method comprises the following specific steps:
at room temperature, 1.22g of Na 2 SiO 3 Added to 30.0g of deionized water, dissolved with stirring, and then added with 11.8g of n-propanol. Stirring vigorously for 1min, and standing for 5min to obtain a propanol-sodium silicate aqueous two-phase system; adding 2.2g of ethyl acetate into the obtained solution, sealing and standing for 2h, filtering the obtained white precipitate, washing the white precipitate with deionized water to neutrality, washing the white precipitate with ethanol once, then placing the white precipitate in a forced air drying oven, and drying the white precipitate for 12h at 60 ℃ to obtain SiO 2 And (3) microspheres.
As shown in FIG. 2, siO was obtained 2 The surface of the microsphere is smooth, and the average grain diameter is 1-2 mu m.
EXAMPLE III
The method for preparing the amphoteric oxide microspheres by the aqueous two-phase system is basically the same as the method in examples 1 and 2, and is different in that the method comprises the following specific steps:
at room temperature, 10mL of self-made sodium zincate solution was taken, and 10g of deionized water and 26.7g of ethanol were added. Stirring vigorously for 1min, standing for 5min to obtain ethanol-sodium zincate aqueous two-phase system; adding 5.5g of ethyl acetate into the obtained solution, sealing and standing for 2h, filtering the obtained white precipitate, washing the white precipitate with deionized water to be neutral, then washing the white precipitate with ethanol once, then placing the white precipitate in a forced air drying oven, and drying the white precipitate for 12h at 60 ℃ to obtain the ZnO microspheres.
As shown in FIG. 3, the obtained ZnO is flower-like microsphere composed of nanosheets, and the average particle size is 7-8 μm.
Example four
The method for preparing the amphoteric oxide microspheres by the aqueous two-phase system is basically the same as that in examples 1-3, and is different in that the method comprises the following specific steps:
at room temperature, 10mL of self-made sodium zincate solution was taken, and 15.3g of deionized water and 21.4g of ethanol were added. Stirring vigorously for 1min, standing for 5min to obtain ethanol-sodium zincate aqueous two-phase system; adding 5.5g of ethyl acetate into the obtained solution, then sealing and standing for 2h, filtering the obtained white precipitate, washing the white precipitate to be neutral by using deionized water, then washing the white precipitate by using ethanol once, then placing the white precipitate in a forced air drying oven, and drying the white precipitate for 12h at the temperature of 60 ℃ to obtain the ZnO microspheres.
As shown in FIG. 3, the obtained ZnO is flower-like microsphere composed of nanosheets, and the average particle size is 4-5 μm.
EXAMPLE five
The method for preparing the amphoteric oxide microspheres by the aqueous two-phase system is basically the same as that in examples 1-4, and is different in that the method comprises the following specific steps:
at room temperature, 10mL of self-made sodium zincate solution was taken, and 25.3g of deionized water and 11.4g of ethanol were added. Stirring vigorously for 1min, standing for 5min to obtain ethanol-sodium zincate aqueous two-phase system; adding 5.5g of ethyl acetate into the obtained solution, then sealing and standing for 2h, filtering the obtained white precipitate, washing the white precipitate to be neutral by using deionized water, then washing the white precipitate by using ethanol once, then placing the white precipitate in a forced air drying oven, and drying the white precipitate for 12h at the temperature of 60 ℃ to obtain the ZnO microspheres.
As shown in FIG. 3, the obtained ZnO microspheres had smooth surfaces and average particle diameters of 0.4 to 0.6. Mu.m.
Table 1 examples 1 to 5
EXAMPLE six
The method for preparing the amphoteric oxide microspheres by the aqueous two-phase system is basically the same as that in examples 1-5, and is different in that the method comprises the following specific steps of:
a method for preparing amphoteric oxide microspheres in a mild manner by using an aqueous two-phase system comprises the following steps:
s1, adding 2.2g of ethyl acetate into precursor liquid of amphoteric oxide salt-small molecular alcohol at room temperature, stirring to form a two-aqueous-phase system, wherein the amphoteric oxide salt precursor solution is an aqueous solution of sodium stannate, sodium silicate and self-made sodium zincate, the small molecular alcohol is absolute ethyl alcohol and propyl alcohol, the using amount of the amphoteric oxide salt is 0.5g, and H in the two-aqueous-phase system 2 The mass of O is 10g, and the mass of alcohol is 11.4g;
s2, carrying out double hydrolysis reaction on the double aqueous phase system obtained in the step S1 to generate white precipitate, wherein sealing operation is required during the double hydrolysis reaction, the hydrolysis temperature is 24 ℃, the hydrolysis time is 2 hours, and the double hydrolysis reaction is carried out under the condition of standing;
s3, filtering the white precipitate obtained in the step S2, and washing with deionized water and absolute ethyl alcohol in sequence;
s4, drying the washed white precipitate in the step S3 to obtain amphoteric oxide microspheres, wherein the drying temperature is set to be 60 ℃, and the drying time is 12h to obtain SnO 2 The average grain diameter of the microspheres is 0.2 mu m, and the prepared SiO 2 The average grain diameter of the microspheres is 1 μm, and the average grain diameter of the prepared ZnO microspheres is 0.4 μm.
EXAMPLE seven
The method for preparing the amphoteric oxide microspheres by the aqueous two-phase system is basically the same as the method in examples 1-6, and is different in that the method comprises the following specific steps:
a method for preparing amphoteric oxide microspheres in a mild manner by using an aqueous two-phase system comprises the following steps:
s1, at room temperature, adding 5.5g of ethyl acetate into precursor liquid of amphoteric oxide salt-small molecular alcohol, stirring to form a two-aqueous-phase system, wherein the amphoteric oxide salt precursor solution is an aqueous solution of sodium stannate, sodium silicate and self-made sodium zincate, the small molecular alcohol is absolute ethyl alcohol and propyl alcohol, the using amount of the amphoteric oxide salt is 1.22g, and H in the two-aqueous-phase system 2 The mass of O is 30g, and the mass of alcohol is 26.7g;
s2, carrying out double hydrolysis reaction on the double aqueous phase system obtained in the step S1 to generate white precipitate, wherein sealing operation is required during the double hydrolysis reaction, the hydrolysis temperature is 26 ℃, the hydrolysis time is 2 hours, and the double hydrolysis reaction is carried out under the condition of standing;
s3, filtering the white precipitate obtained in the step S2, and washing with deionized water and absolute ethyl alcohol in sequence;
s4, drying the washed white precipitate in the step S3 to obtain amphoteric oxide microspheres, wherein the drying temperature is set to be 62 ℃, and the drying time is 15h to prepare the prepared SnO 2 The average grain diameter of the microspheres is 1 mu m, and the prepared SiO 2 The average grain diameter of the microspheres is 2 mu m, and the average grain diameter of the prepared ZnO microspheres is 8 mu m.
The method for preparing the amphoteric oxide microspheres mildly by the double-aqueous-phase system provided by the embodiment of the invention has the advantages that green raw materials of micromolecule alcohol and ethyl acetate participate in product synthesis, the operation is simple and convenient, the cost is low, meanwhile, the method has certain universality, ideas are provided for preparing amphoteric oxides from alkaline salt solutions and expanding a liquid-phase precipitation system to the double-aqueous-phase system, a general method for preparing the amphoteric oxides from the alkaline salt solutions is developed by using different precursor solutions and ethyl acetate in a matching manner, the repeatability is good, the synthesized amphoteric oxide materials such as ZnO and the like have good application potential in the fields of gas sensors, batteries, catalysis and the like, the precipitation rate can be controlled by controlling the system interface condition (alcohol consumption) through an auxiliary synthesis strategy of the salt-alcohol double-aqueous-phase system, the product morphology is further regulated, and the diffusion rate of reaction particles is controlled by the phase interface condition through the double-aqueous-phase system of the amphoteric oxide acid salt-micromolecule alcohol, so that the precipitation rate is reduced, and the amphoteric oxide microspheres with uniform particle sizes are obtained.
The key point of the above embodiment of the present invention is that the double aqueous phase system of amphoteric oxysalt-small molecular alcohol realizes the control of the diffusion rate of the reaction particles under the condition of phase interface, so as to reduce the precipitation rate and obtain amphoteric oxide microspheres with uniform particle size; the precipitation strategy takes small molecular alcohol, ethyl acetate and other green raw materials to participate in product synthesis, and has simple and convenient operation and low cost; meanwhile, the method has certain universality, and provides a new technical idea for preparing amphoteric oxide from alkaline salt solution and expanding a liquid-phase precipitation system to a two-aqueous-phase system.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A method for preparing amphoteric oxide microspheres by a two-aqueous-phase system is characterized by comprising the following steps:
s1, adding 2.2-5.5g of ethyl acetate into a precursor liquid of amphoteric oxide acid salt-small molecular alcohol at room temperature, and stirring to form a two-aqueous-phase system;
s2, carrying out double hydrolysis reaction on the double aqueous phase system obtained in the step S1 to generate white precipitate;
s3, filtering the white precipitate obtained in the step S2, and washing with deionized water and absolute ethyl alcohol in sequence;
and S4, drying the washed white precipitate in the step S3 to obtain the amphoteric oxide microspheres.
2. The method for mildly preparing the amphoteric oxide microspheres by using the aqueous two-phase system according to claim 1, wherein in the step S1, the amphoteric oxide salt precursor solution is an aqueous solution of sodium stannate, sodium silicate and self-made sodium zincate, and the small molecular alcohol is absolute ethyl alcohol and propyl alcohol.
3. The method for preparing amphoteric oxide microspheres according to claim 1, wherein in step S1, the amount of amphoteric oxide salt is 0.5-1.22g, and the amount of H in the aqueous two-phase system is 0.5-1.22g 2 The mass of O is 10-30g, and the mass of alcohol is 11.4-26.7g.
4. The method for the mild preparation of amphoteric oxide microspheres according to claim 1, wherein in step S2, the sealing operation with plastic wrap is performed during the double hydrolysis reaction.
5. The method for preparing the amphoteric oxide microspheres by using the aqueous two-phase system according to claim 1, wherein in the step S2, the hydrolysis temperature is 24-26 ℃, and the hydrolysis time is 2 hours.
6. The method for the mild preparation of amphoteric oxide microspheres according to claim 1, wherein in step S2, the double hydrolysis reaction is performed under a standing condition.
7. The method for preparing amphoteric oxide microspheres according to claim 1, wherein in step S4, the prepared SnO 2 The microspheres have an average particle size of 0.2-1 μm.
8. The method for preparing amphoteric oxide microspheres according to claim 1, wherein in step S4, the prepared SiO is 2 Microspheres of flatThe average particle diameter is 1-2 μm.
9. The aqueous two-phase system and the method for preparing amphoteric oxide microspheres according to claim 1, wherein in step S4, the average particle size of the ZnO microspheres prepared is 0.4-8 μm.
10. The method for the mild preparation of amphoteric oxide microspheres according to claim 1, wherein in step S4, the temperature during drying is set to 60-62 ℃ and the drying time is 12-15h.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343043A (en) * | 2008-08-25 | 2009-01-14 | 中国科学院上海硅酸盐研究所 | Amphoteric metal compound nano-material and method of preparing the same |
| US20100008847A1 (en) * | 2006-12-21 | 2010-01-14 | Dunbar Timothy D | Process for producing nanoparticles |
| JP2015110503A (en) * | 2013-04-19 | 2015-06-18 | 住友大阪セメント株式会社 | Silicon oxide-coated zinc oxide and production method of the same, silicon oxide-coated zinc oxide-containing composition, and cosmetic |
| CN110240193A (en) * | 2019-07-01 | 2019-09-17 | 广州大学 | A kind of amphoteric metal oxidate microspheres and its preparation method and application |
-
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- 2022-06-23 CN CN202210716928.4A patent/CN115159563A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100008847A1 (en) * | 2006-12-21 | 2010-01-14 | Dunbar Timothy D | Process for producing nanoparticles |
| CN101343043A (en) * | 2008-08-25 | 2009-01-14 | 中国科学院上海硅酸盐研究所 | Amphoteric metal compound nano-material and method of preparing the same |
| JP2015110503A (en) * | 2013-04-19 | 2015-06-18 | 住友大阪セメント株式会社 | Silicon oxide-coated zinc oxide and production method of the same, silicon oxide-coated zinc oxide-containing composition, and cosmetic |
| CN110240193A (en) * | 2019-07-01 | 2019-09-17 | 广州大学 | A kind of amphoteric metal oxidate microspheres and its preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| BIN WEN等: ""Preparation of the Silica Micro-Spheres by Chemical Precipitation Process"", 《ADVANCED MATERIALS RESEARCH》, vol. 602, pages 259 - 264 * |
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