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Method for preparing nano SiO2 through microemulsion online monitoring process

A microemulsion and nanotechnology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of long cycle, cumbersome experiments, and inability to diagnose in time, and achieve good dispersion and particle size. Controllable, narrow particle size distribution effect

Inactive Publication Date: 2018-10-09
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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Problems solved by technology

But only through the final characterization, there is no way to know the changes in the experimental process, which makes it impossible to diagnose the cause of the experimental failure in time, making the experiment cumbersome and the cycle longer

Method used

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  • Method for preparing nano SiO2 through microemulsion online monitoring process

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Experimental program
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Effect test

Embodiment 1

[0016] a. Prepare cyclohexane: OP-10: n-butanol (molar ratio) = 38:1:2.5 mixed solution, slowly add 104 mmol ammonia water to the above mixed solution, set the speed at 3000 rpm and the temperature at 20 ℃, mix 2 hours to get translucent microemulsion

[0017] b. Add 156 mmol orthoethyl silicate (TEOS) into the microemulsion in step a, react for 2 hours, age for 10 hours, wash, separate, and dry for 4 hours to obtain SiO with a particle size of 150 nm 2 .

Embodiment 2

[0019] a. Prepare cyclohexane: OP-10: n-butanol (molar ratio) = 76:1:2.5 mixed solution, slowly add 260 mmol ammonia water to the above mixed solution, set the speed at 4000 rpm and the temperature at 30°C, mix 2 hours to get a translucent microemulsion

[0020] b. Add 390 mmol tetraethyl orthosilicate (TEOS) into the microemulsion in step a, react for 4 hours, age for 10 hours, wash, separate, and dry for 4 hours to obtain SiO with a particle size of 50 nm 2 .

Embodiment 3

[0022] a. Prepare cyclohexane: OP-10: n-butanol (molar ratio) = 114:1:2.5 mixed solution, slowly add 416 mmol ammonia water to the above mixed solution, set the speed at 5000 rpm and the temperature at 40 ℃, mix 2 hours to get translucent microemulsion

[0023] b. Add 642 mmol tetraethyl orthosilicate (TEOS) into the microemulsion in step a, react for 5 hours, age for 10 hours, wash, separate, and dry for 6 hours to obtain SiO with a particle size of 400 nm 2 .

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Abstract

The invention discloses a method for preparing nano SiO2 through a microemulsion online monitoring process. The method includes: preparing nano SiO2 through the microemulsion process; adopting an online granularity analysis system to continuously monitor change of particle diameter of SiO2 particles; analyzing changing tendency of characteristics of the nano SiO2 particles within 24h, like granularity and number to regulate size of microemulsion balls and hydration particle diameter of nano SiO2. SiO2 prepared by the method is controllable in particle diameter, narrow in distribution and highin dispersity, and average particle diameter of SiO2 is within a range of 50-400nm.

Description

technical field [0001] The invention relates to the field of preparation of inorganic non-metallic nanomaterials, in particular to a microemulsion on-line monitoring method for preparing nano-SiO 2 Methods. Background technique [0002] Traditionally, the prepared samples need to be analyzed by specialized testers and the data is fed back to the experimenters, and then adjustments are made according to the results. For nano-SiO 2 The mentioned characterizations are usually also performed using several off-line analytical tools including optical analysis (optical microscopy, scanning electron microscopy (SEM)), thermal analysis (differential scanning calorimetry (DSC), thermogravimetric analysis (TG)), Vibrational spectroscopy (Fourier transform infrared spectroscopy, Raman spectroscopy, solid-state nuclear magnetic resonance (ssNMR) and X-ray diffraction (XRD)). But only through the final characterization, there is no way to know the changes in the experimental process, w...

Claims

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Application Information

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IPC IPC(8): C01B33/18B82Y30/00B82Y40/00
CPCC01B33/18B82Y30/00B82Y40/00C01P2004/62C01P2004/64
Inventor 刘玉敏齐然张志昆刘越顾春雷张向京
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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