CN111943216A - Electric field reinforced dispersed nano SiO2Process for the preparation of granules - Google Patents

Electric field reinforced dispersed nano SiO2Process for the preparation of granules Download PDF

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Publication number
CN111943216A
CN111943216A CN202010714518.7A CN202010714518A CN111943216A CN 111943216 A CN111943216 A CN 111943216A CN 202010714518 A CN202010714518 A CN 202010714518A CN 111943216 A CN111943216 A CN 111943216A
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China
Prior art keywords
solution
lysine
beaker
electric field
sio
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CN202010714518.7A
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Chinese (zh)
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颜伟城
王建
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Jiangsu University
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Jiangsu University
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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
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • 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
    • 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
    • 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
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • 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
    • C01P2004/52—Particles with a specific particle size distribution highly monodisperse 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

Abstract

The invention belongs to the technical field of nano material synthesis, and particularly relates to electric field reinforced dispersion nano SiO2A method for preparing the particles. The method comprises the steps of firstly preparing a lysine solution, controlling the flow rate of the lysine solution by using an injection pump, atomizing the lysine solution by using a high-voltage power supply, heating and collecting the lysine solution in water bath by using a beaker filled with a TEOS solution, and finally drying the solution at 60 ℃ to obtain SiO2-n. The invention expands the application range of the electrostatic spraying process; meanwhile, the method can be used for continuous preparation, and has practical significance for industrial production.

Description

Electric field reinforced dispersed nano SiO2Process for the preparation of granules
Technical Field
The invention belongs to the technical field of nano material synthesis, and particularly relates to electric field reinforced dispersion nano SiO2A method for preparing the particles.
Background
Silica is not only a raw material for manufacturing parts of optical instruments and electronic products, but also a good catalyst carrier. SiO 22And-n has wide application prospect in the fields of catalysis, optics, magnetic media and new materials due to the special properties of small-size effect, surface effect and the like.
From the beginning of the 20 th century, researchers have conducted research into electrohydrodynamic atomization (also known as electrostatic spraying). Since the 21 st century, electrostatic spraying technology has been extensively applied and used for preparing micro-nano particles due to its advantages of simplicity, controllability and high efficiency. The conventional preparation methods such as sol-gel method, precipitation method and the like can also prepare SiO2N, but the process is an inefficient, complex, cumbersome batch operation.Based on the defects of intermittent operation and along with the increasing maturity of electrostatic spraying technology, the nano SiO with electric field strengthening dispersion needs to be provided2The preparation method of the particles is to use the combination of an electrostatic spraying device and a constant-temperature magnetic stirring device to carry out continuous operation to prepare SiO2-n。
Disclosure of Invention
The invention aims to provide a simple and controllable electric field strengthening method for preparing SiO by continuous operation2-n.
The method comprises the steps of firstly preparing a lysine solution, controlling the flow rate of the lysine solution by using an injection pump, atomizing the lysine solution by using a high-voltage power supply, heating and collecting the lysine solution in water bath by using a beaker filled with a TEOS solution, and finally drying the solution at 60 ℃ to obtain SiO2-n。
SiO specific to the invention2-n is prepared according to the following steps:
in the first step, L-lysine is weighed and dissolved in a mixed solvent of distilled water and cyclohexane to obtain a lysine mixed solution.
And secondly, fixing the syringe for absorbing the lysine solution on an injection pump, and fixing the needle head and the high-pressure generating device.
And thirdly, placing the beaker filled with the TEOS solution on a constant-temperature magnetic stirring device, controlling the water bath temperature at 50-70 ℃, and fully stirring the TEOS solution.
And fourthly, carrying out grounding treatment on the beaker filled with the TEOS solution by using tinfoil to prevent electric shock.
Fifthly, setting a syringe pump, controlling the flow rate of the lysine solution to be 3-9ml/h, and starting the syringe pump to inject.
And sixthly, starting a high-voltage power supply, adjusting the voltage, and atomizing the lysine solution and feeding the lysine solution into a beaker filled with the TEOS solution.
And seventhly, after the injection of the injection pump is finished, fully stirring the mixed solution in the beaker, and stopping the experiment.
Eighthly, putting the beaker into a drying oven for drying, and lightly scraping off the powder deposited at the bottom of the beaker after the beaker is completely driedThus obtaining SiO2-n。
In the first step, the ratio of lysine to the mixed solvent of distilled water and cyclohexane was 1.168 g: 147.7 mL; the volume ratio of distilled water to cyclohexane was 139: 8.7.
the ratio of the volume of lysine solution sucked from the syringe in the second step to the volume of TEOS solution purchased from Chinese medicine in the third step was 6.65:5 (80124118).
In the seventh step, the time for sufficient stirring is 1 h.
In the eighth step, the drying temperature was 60 ℃.
SiO in the invention2The surface morphology and structure information of-n are obtained by Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM), and the particle size distribution is measured by a Malvern nanometer laser particle sizer.
Advantageous effects
Provides a nano SiO with electric field strengthening dispersion2The particle preparation method enables the electrostatic spraying device to be combined with other devices, thereby expanding the application range of the electrostatic spraying process; meanwhile, the method can be used for continuous preparation, and has practical significance for industrial production.
Drawings
FIG. 1 is a diagram of an experimental setup, labeled as follows: (a) a high voltage power supply; (b) a needle cylinder; (c) an injection pump; (d) a needle head; (e) a beaker; (f) grounding the tinfoil; (g) a constant temperature magnetic stirrer.
FIG. 2 is SiO2N surface topography and internal structure diagram, which are labeled as follows: (a) - (b) is SiO2-SEM of n; (c) - (d) is SiO2-n of TEM.
Prepared SiO2The morphology of the-n is spherical, the size is about 40nm, and the shape is uniform.
FIG. 3 is SiO2-a particle size distribution map of n.
The particle size distribution profile also shows that the particles have a better uniformity, following a normal distribution.
FIG. 4 is SiO2-eds plot of n.
Theoretically, the atomic ratio of O atoms to Si atoms is 2, and as shown in fig. 4 is 1.98, very close.
Detailed Description
The invention is described in detail below with reference to the example drawings so that those skilled in the art can better understand the invention.
(1) First, 1.168g L-lysine was weighed and dissolved in a mixed solvent of 139ml of distilled water and 8.7ml of cyclohexane to obtain a lysine mixed solution.
(2) And (3) sucking the lysine solution by using a syringe, then fixing the syringe for sucking the lysine solution on a syringe pump, and fixing the needle head with the high-pressure generating device.
(3) The beaker containing 5ml TEOS solution is placed on a constant temperature magnetic stirring device, the water bath temperature is 50, 55, 60, 65 and 70 ℃, and the solution can be ensured to be fully stirred.
(4) And the bottom of the beaker is grounded by using tinfoil to prevent electric shock.
(5) Setting a syringe pump, setting the total injection amount of the lysine solution to be 6.65ml and the flow rate to be 3, 5, 7 and 9ml/h respectively, and starting the syringe pump to inject.
(6) And starting a high-voltage power supply to regulate the voltage, so that the lysine solution is atomized and enters a beaker filled with the TEOS solution.
(7) After the injection of the injection pump was completed, the mixed solution in the beaker was stirred sufficiently for one hour to stop the experiment.
(8) Drying the beaker in a drying oven at 60 ℃, and slightly scraping the powder deposited at the bottom of the beaker after the beaker is completely dried to obtain the SiO2-n。
(9) SiO prepared under different conditions2N conducting a nanometer laser particle sizer test to count the particle size distribution.

Claims (5)

1. Electric field reinforced dispersed nano SiO2The preparation method of the granules is characterized by preparing a lysine solution, controlling the flow rate of the lysine solution by using an injection pump, atomizing the lysine solution by using a high-voltage power supply, heating and collecting the lysine solution in water bath by using a beaker filled with a TEOS solution, and finally drying the solution at 60 ℃ to obtain SiO2N, the specific steps are as follows:
firstly, weighing L-lysine, and dissolving the L-lysine in a mixed solvent of distilled water and cyclohexane to obtain a lysine mixed solution;
secondly, the syringe for absorbing the lysine solution is placed on an injection pump to be fixed, and the needle head is fixed with a high-pressure generating device;
thirdly, placing the beaker filled with the TEOS solution on a constant-temperature magnetic stirring device, controlling the water bath temperature at 50-70 ℃, and fully stirring the TEOS solution;
fourthly, carrying out grounding treatment on the beaker filled with the TEOS solution by using tinfoil to prevent electric shock;
fifthly, setting an injection pump, controlling the flow rate of the lysine solution to be 3-9ml/h, and starting the injection pump for injection;
sixthly, starting a high-voltage power supply, and adjusting the voltage to atomize the lysine solution and feed the lysine solution into a beaker filled with the TEOS solution;
seventhly, after the injection of the injection pump is finished, fully stirring the mixed solution in the beaker, and stopping the experiment;
eighthly, putting the beaker into a drying oven for drying, and slightly scraping the powder deposited at the bottom of the beaker after the beaker is completely dried to obtain the SiO2-n。
2. The electric field enhanced dispersed nano SiO of claim 12A process for producing pellets, characterized in that, in the first step, the ratio of lysine to a mixed solvent of distilled water and cyclohexane is 1.168 g: 147.7 mL; the volume ratio of distilled water to cyclohexane was 139: 8.7.
3. the electric field enhanced dispersed nano SiO of claim 12The granule preparation method is characterized in that the volume ratio of the lysine solution sucked in the syringe in the second step to the TEOS solution in the third step is 6.65: 5.
4. The electric field enhanced dispersed nano SiO of claim 12A process for the preparation of granules, characterized in that,in the seventh step, the time for sufficient stirring is 1 h.
5. The electric field enhanced dispersed nano SiO of claim 12The process for producing granules, wherein in the eighth step, the drying temperature is 60 ℃.
CN202010714518.7A 2020-07-23 2020-07-23 Electric field reinforced dispersed nano SiO2Process for the preparation of granules Pending CN111943216A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114988466A (en) * 2022-05-20 2022-09-02 佛山(华南)新材料研究院 Mesoporous TiO with high tap density 2 Microspheres and method for preparing same

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104609431A (en) * 2015-01-19 2015-05-13 武汉金弘扬化工科技有限公司 Synthetic method and particle size control synthetic method for SiO2 nano particles smaller than 50 nm
CN206464101U (en) * 2016-12-08 2017-09-05 东华理工大学 A kind of drop induc- tion charging atomization test device
CN107416849A (en) * 2017-09-06 2017-12-01 青岛科技大学 A kind of method for preparing monodisperse nano silicon dioxide particle

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104609431A (en) * 2015-01-19 2015-05-13 武汉金弘扬化工科技有限公司 Synthetic method and particle size control synthetic method for SiO2 nano particles smaller than 50 nm
CN206464101U (en) * 2016-12-08 2017-09-05 东华理工大学 A kind of drop induc- tion charging atomization test device
CN107416849A (en) * 2017-09-06 2017-12-01 青岛科技大学 A kind of method for preparing monodisperse nano silicon dioxide particle

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114988466A (en) * 2022-05-20 2022-09-02 佛山(华南)新材料研究院 Mesoporous TiO with high tap density 2 Microspheres and method for preparing same
CN114988466B (en) * 2022-05-20 2024-04-09 佛山(华南)新材料研究院 Mesoporous TiO with high tap density 2 Microsphere and preparation method thereof

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