Manufacturing method of silica sol and obtained silica sol

A manufacturing method and technology of silica sol, which is applied in the field of silica sol, can solve the problems of limited particle size of silica sol, high performance requirements of production equipment, uneven particle size, etc., and achieve low equipment performance requirements, low cost, and good uniformity Effect

Inactive Publication Date: 2006-09-13
SHANGHAI INST OF APPLIED PHYSICS - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are deficiencies in these processes: the particle size of the silica sol prepared by the high temperature and high pressure method is very limited, and the particle size is not uniform. For example, the preparation of a silica sol with an average particle diameter of about 20 nm requires a pressure of 10 to 15 atmospheres. And the water temperature of nearly 160-180 ℃; and high performance requirements for production equipment, high energy consumption, and a large number of concentration steps in the later stage; the method of adding active silicic acid particles to the seed liquid avoids high temperature and high pressure, and requires high equipment performance. Low, and can prepare silica sol with relatively large particles
However, in these methods of using silica powder as the main raw material to prepare silica sol, the particles of the prepared silica sol are all low, and it is difficult to meet the requirements for preparing higher-grade silica sol, such as silica sol for semiconductor chip polishing, etc.

Method used

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  • Manufacturing method of silica sol and obtained silica sol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a 2000 ml four-neck flask equipped with a reflux device, dilute 200 g of silica sol with a solid content (silica particles) of 30% (mass) and a particle diameter of 40 to 50 nm with 1000 ml of water to SiO 2The mass concentration is about 5%. Stirring and heating are started, and another 6g of NaOH solid is weighed and dissolved with a small amount of water to form a solution with a concentration of about 10%. When the temperature rises to 85°C, start to add the commercially available 200-300 mesh silicon powder while adding the NaOH solution. NaOH was added at a rate to keep the pH of the system in the range of 9.0 to 10.0; the silicon powder was added at a rate to keep the reaction temperature not exceeding 90° C., and a total of 220 g (catalyst: silicon powder=1:37) silicon powder was added. After adding all the NaOH and silicon powder, keep the temperature and react for 5 hours, then keep stirring, cool to below 60°C and filter. The obtained silica sol index is ...

Embodiment 2

[0027] Using the same conditions as in Example 1, the difference is: the use of solid content is 20%, and the particle diameter is 300g of silica sol diluted to SiO with 10000 milliliters of water. 2 The mass content is about 0.6%; NaOH is dissolved in water to make the concentration about 2% before adding. Finally obtained silica sol index is as follows:

[0028] SiO 2 Mass content: 3.0% SiO 2 Particle size: 5~20nm

[0029] Viscosity (20°C): 1.4mp a ·s Silica fume utilization rate: 80%

Embodiment 3

[0031] Using the same conditions as in Example 1, the difference is: using silica sol with a particle size of 10-15 nm as the seed liquid; dissolving NaOH in water to a concentration of about 20% before adding. Finally obtained silica sol index is as follows:

[0032] SiO 2 Mass content: 35.0% SiO 2 Particle size: 20~30nm

[0033] Viscosity (20°C): 10.5mp a ·s Silica fume utilization rate: 89%

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Abstract

A process for preparing high-granularity Si sol includes such steps as heating the SiO2 dispersed water, stirring while adding alkaline catalyst and metallic Si powder, hydrolytic reaction at pH=7-14 to obtain active silicic acid micro-particles, and quickly adsorbing the micro-particles by SiO2 seed particles to become target sol. Its advantages are high speed and controllable and uniform granularity.

Description

technical field [0001] The invention relates to a method for producing silica sol and the silica sol prepared therefrom. Background technique [0002] At present, there are generally the following methods for producing large-size silica sol in industry. One is the method of adopting high temperature and high pressure method in the ion exchange process and adding active silicic acid raw materials dropwise while heating and evaporating on the basis of seed liquid. Such as U.S. patents: US3012972 (1962), US4356107 (1982), are to use high temperature and high pressure to process alkaline small particle size silica sol in order to obtain large particle size silica sol; patent US3947376 (1976), US4304575 (1981) and China The patent CN1155514A (1997) basically adopts silicon dioxide with a certain particle size as the seed liquid, and then adopts the method of adding active silicic acid microparticles dropwise while heating and evaporating to obtain a silica sol with a large parti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/14C01B33/141
Inventor 许念强顾建祥罗康郑松保
Owner SHANGHAI INST OF APPLIED PHYSICS - CHINESE ACAD OF SCI
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