A method for continuous and controllable preparation of nano-silica spherical particles

A technology of nano-silica and silicon oxide particles, which is applied in the direction of silica, silicon oxide, nanotechnology, etc., can solve the problems of high cost and complicated operation, and achieve high production efficiency, simple post-processing, and high yield Effect

Active Publication Date: 2021-03-09
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method is complex and expensive

Method used

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  • A method for continuous and controllable preparation of nano-silica spherical particles
  • A method for continuous and controllable preparation of nano-silica spherical particles
  • A method for continuous and controllable preparation of nano-silica spherical particles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 528g of methyl orthosilicate and 660g of methanol into a 2L beaker, and stir for 30min to form solution A; then add 247.5g of deionized water, 412.5g of sodium hydroxide (30wt%) and 528g of methanol into a 2L beaker, and stir for 30min Solution B is formed. The prepared two cups of solutions A and B are pumped into the T-shaped microchannel mixer by the metering pump at the same time. The feeding angle of the two liquids is 90 degrees. The inner diameter of the microchannel used is 0.68mm and the length of the microchannel is 60cm. At this time, the microwave controlled heating temperature was 98° C., and the heating residence time was 1 h. After solid-liquid separation, the product was placed in a constant temperature and humidity box at a temperature of 85°C and a humidity of 90%, and dried for 12 hours.

[0036] Gained product analyzes particle size with Malvern laser particle size analyzer, and its average particle diameter is 209.3nm, and concentration PDI val...

Embodiment 2

[0038] Add 733.2g of tetraethyl orthosilicate and 670.8g of isopropanol into a 2L beaker, and stir for 30min to form solution A; then add 351g of deionized water, 382.2g of concentrated ammonia water and 670.8g of isopropanol into a 2L beaker, and stir Solution B was formed in 30 min. The prepared two cups of solutions A and B are pumped into the T-shaped microchannel mixer by the metering pump at the same time. The feeding angle of the two liquids is 90 degrees. The inner diameter of the microchannel used is 1mm and the length of the microchannel is 16cm. At this time, the microwave controlled heating temperature was 120° C., and the heating residence time was 0.5 h. After solid-liquid separation, the product was placed in a constant temperature and humidity box at a temperature of 90°C and a humidity of 50%, and dried for 18 hours.

[0039]Gained product analyzes particle size with Malvern laser particle size analyzer, and its average particle diameter is 138.7nm, and conce...

Embodiment 3

[0041] Add 72.5g of methyl orthosilicate and 971.5g of ethanol into a 2L beaker, and stir for 30min to form solution A; then add 580g of deionized water, 290g of concentrated ammonia water and 174g of isopropanol into a 2L beaker, and stir for 30min to form solution B . The prepared two cups of solutions A and B are pumped into the T-shaped microchannel mixer by the metering pump at the same time. The feeding angle of the two liquids is 90 degrees. The inner diameter of the microchannel used is 0.8mm and the length of the microchannel is 40cm. At this time, the microwave controlled heating temperature was 78° C., and the heating residence time was 2 h. After solid-liquid separation, the product was placed in a constant temperature and humidity box at a temperature of 90°C and a humidity of 50%, and dried for 24 hours.

[0042] Gained product analyzes particle size with Malvern laser particle size analyzer, and its average particle diameter is 27.45nm, and concentration PDI va...

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Abstract

The invention provides a method for continuously and controllably preparing nano-silica spherical particles, which comprises the following steps: using alcohol as a dispersant, organosilicon and silicate as a silicon source, and hydrolyzing under the action of an alkaline catalyst to obtain nano-dioxide Silicon spherical particles are then dried to obtain a solid product. The preparation process mainly includes: simultaneously introducing the silicon source solution and the catalyst into the microchannel mixer to strengthen the mixing, then heating to a certain temperature with high intensity, and after a certain time of aging reaction, the finished nano-silica products of different scales can be directly obtained. particles. The characteristics of the method of the invention are: high-purity silica particles with a particle size of 10-1000 nm, high sphericity, and a uniformity PDI range of 0.02-0.3 can be prepared, and the method of the invention has high efficiency, uniform product particles, and nano-scale. Controllable, high yield, easy to scale up and can realize continuous production.

Description

technical field [0001] The invention relates to the field of material preparation, in particular to a method for continuously and controllably preparing spherical nanoparticles of silicon dioxide. Background technique [0002] The synthesis of monodisperse SiO2 particles has attracted much attention in the field of materials, and its monodisperse particles can self-assemble into new multifunctional materials, which can be adapted to special applications in different fields. Precise control of the size of SiO2 monodisperse particles has a decisive impact on the later assembly and synthesis of new composite materials. In the past 30 years, many scholars have devoted themselves to the development and improvement of technologies for synthesizing different scales. Nano-silica materials are widely used in industrial fields: catalysts, stabilizers, polishing powders, coatings, drug carriers, adsorption and separation materials, etc. The size and uniformity of its size are the key ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/18B82Y40/00
CPCC01B33/18C01P2004/03C01P2004/04C01P2004/32C01P2004/52C01P2004/62C01P2004/64
Inventor 苏宏久任高远王树东
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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