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CN1273381C - Method for preparing submicro and nano silicon dioxide in spherical shape - Google Patents

Method for preparing submicro and nano silicon dioxide in spherical shape Download PDF

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Publication number
CN1273381C
CN1273381C CN 200410012854 CN200410012854A CN1273381C CN 1273381 C CN1273381 C CN 1273381C CN 200410012854 CN200410012854 CN 200410012854 CN 200410012854 A CN200410012854 A CN 200410012854A CN 1273381 C CN1273381 C CN 1273381C
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CN
China
Prior art keywords
preparation
silicon dioxide
preparing
submicron
dioxide
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Expired - Fee Related
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CN 200410012854
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Chinese (zh)
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CN1562742A (en
Inventor
袁良杰
李明
孙聚堂
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Wuhan University WHU
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Wuhan University WHU
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Priority to CN 200410012854 priority Critical patent/CN1273381C/en
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Publication of CN1273381C publication Critical patent/CN1273381C/en
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Abstract

The present invention discloses a method for preparing spherical submicron and nanometer silicon dioxide. Potassium silicate containing 1 to 20 wt% of silicon dioxide, sodium silicate, or alkaline silicon collosol and 1 to 20 wt% of sulphuric acid are respectively and continuously introduced into a reaction vessel according to the flow rate of 1 to 300 L/min. The materials are stirred to maintain turbulent flow circulation for 1 to 100 minutes, and separated after being made to stand and cured. Aproduct is washed with deionized water at 25 to 100 DEG C until the pH value reaches 5 to 7, and spherical submicron and nanometer silicon dioxide with the particle size of 5 to 10 nm is prepared. The preparation method has the advantages of simple technological process and low energy consumption. The ratio surface of a product can be controlled by heating temperature. The product has the advantages of high purity, good fluidity, easy dispersion and controllable particle size between 5 and 10 nm. The method is suitable for preparing an encapsulation material of great-scale integrated circuit,and the method also can be used for the fields of machine, electron, chemical engineering, biological medicine, etc.

Description

The preparation method of submicron and nanometer spherical silicon-dioxide
Technical field
The present invention relates to the preparation method of a kind of submicron and nanometer spherical silicon-dioxide, belong to inorganic new material technology field.
Background technology
Submicron and nanometer spherical silicon-dioxide can be used for the encapsulating compound preparation of super large-scale integration, also can be used for fields such as machinery, electronics, daily-use chemical industry, biological medicine.
According to bibliographical information, the method for existing submicron and nanometer spherical silicon-dioxide mainly contains following several: 1, obtaining behind the silicon sol again by potassium silicate (sodium) and acid-respons, high-temperature injection prepares submicron and nanometer spherical silicon-dioxide; 2, organosilicon hydrolyzation prepares submicron and nanometer spherical silicon-dioxide; 3, the revaporization oxidation formed submicron and nanometer spherical silicon-dioxide after silica at high temperature was reduced into silicon monoxide; 4, the direct high-temperature evaporation-condensation of titanium dioxide silico briquette prepares submicron and nanometer spherical silicon-dioxide; 5, the organosilicon spray burning prepares submicron and nanometer spherical silicon-dioxide; 6, microemulsion method prepares submicron and nanometer spherical silicon-dioxide.Because aforesaid method adopts vaporization under high-temperature injection, organosilicon hydrolyzation, the high temperature, spray burning or microemulsion method etc., its preparation is complicated, energy consumption is high.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides the preparation method of a kind of submicron and nanometer spherical silicon-dioxide.This method mild condition, technological process is simple, products obtained therefrom good fluidity, good dispersity, controllable specific surface area.
For realizing that the technical measures that purpose of the present invention is taked are:
A kind of method for preparing submicron and nanometer spherical silicon-dioxide, to contain potassium silicate, water glass or the alkaline silica sol of silica 1~20wt% and the sulfuric acid of 1~20wt% and import reaction vessel continuously by 0.5~50mL/min flow respectively, stirring allows material keep turbulent flow circulation 1~100min, and separate still aging back; To pH 5~7, oven dry promptly gets granularity 5 μ m~10nm submicron and nanometer spherical silicon-dioxide with 25~100 ℃ deionized water wash products.
According to technical scheme of the present invention, still aging time 10~600min.
According to technical scheme of the present invention, bake out temperature is 25 to 500 ℃, 1~10 hour time of drying.
The present invention can carry out surface treatment as required after oven dry, comprise that heating surface is handled and (or) chemical surface treatment.
Wherein the heating surface temperature ranges is 500~1200 ℃; Chemical surface treatment is conventional dry method or wet method surface treatment.
Compared with prior art, the beneficial effect that adopts technical scheme of the present invention and reached:
Preparation method's technological process of the present invention is simple, and energy consumption is low; The product specific surface area can be regulated and control by Heating temperature, the purity height of product, good fluidity, easily disperse, granularity is regulated and control between 5 μ m~10nm, is suitable for the encapsulating compound preparation of super large-scale integration, also can be used for fields such as machinery, electronics, daily-use chemical industry, biological medicine.
Embodiment
Example 1:
Measure the sulphuric acid soln of 1000mL 1.2g/mL water glass and 500mL 20% respectively, import stainless steel vessel with the flow of 1mL/min and 0.5mL/min respectively, and stir still aging time 120min behind the turbulent circulation 60min.Filter, wash pH5~7,120 ℃ dry 2 hours down, obtain 1 micron preparing spherical SiO 2 through 1180 degree processing again with 50 ℃ of deionizations.
Example 2:
Measure the sulphuric acid soln of 1000mL 1.1g/mL alkaline silica sol and 20mL 10% respectively, respectively in the flow feeding reaction device with 50mL/min and 1mL/min, the still aging time 240min of turbulent circulation 90min.Filter,, spend the preparing spherical SiO 2 that processing obtains 70 nanometers through 1200 again with 70 ℃ of deionized water wash ℃ dry 8 hours down to pH5~7,60.
Example 3:
Measure the sulphuric acid soln of 1000mL 1.1g/mL potassium silicate and 500mL 5% respectively, respectively in the flow feeding reaction device with 1mL/min and 0.5mL/min, the still aging time 350min of turbulent circulation 100min.Filter, with 30 ℃ of deionized water wash to pH5~7,200 ℃ dry 1.5 hours down, conventional dry method of process or wet method surface treatment obtained the preparing spherical SiO 2 of 50 nanometers again.

Claims (5)

1. method for preparing submicron and nanometer spherical silicon-dioxide, it is characterized in that: will contain potassium silicate, water glass or the alkaline silica sol of silica 1~20wt% and the sulfuric acid of 1~20wt% and import reaction vessel continuously by 0.5~50mL/min flow respectively, stirring allows material keep turbulent flow circulation 1~100min, and separate still aging back; To pH5~7, oven dry promptly gets granularity 5 μ m~10nm submicron and nanometer spherical silicon-dioxide with 25~100 ℃ deionized water wash products.
2. preparation method according to claim 1 is characterized in that: described still aging time 10~600min.
3. preparation method according to claim 1 and 2 is characterized in that: bake out temperature is 25 to 500 ℃, 1~10 hour time of drying.
4. preparation method according to claim 1 and 2 is characterized in that: carry out surface treatment after the oven dry.
5. preparation method according to claim 4 is characterized in that: surface treatment is that heating surface is handled or chemical surface treatment; Wherein the heating surface temperature ranges is 500~1200 ℃.
CN 200410012854 2004-03-18 2004-03-18 Method for preparing submicro and nano silicon dioxide in spherical shape Expired - Fee Related CN1273381C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 200410012854 CN1273381C (en) 2004-03-18 2004-03-18 Method for preparing submicro and nano silicon dioxide in spherical shape

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 200410012854 CN1273381C (en) 2004-03-18 2004-03-18 Method for preparing submicro and nano silicon dioxide in spherical shape

Publications (2)

Publication Number Publication Date
CN1562742A CN1562742A (en) 2005-01-12
CN1273381C true CN1273381C (en) 2006-09-06

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN 200410012854 Expired - Fee Related CN1273381C (en) 2004-03-18 2004-03-18 Method for preparing submicro and nano silicon dioxide in spherical shape

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CN (1) CN1273381C (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100447081C (en) * 2005-09-15 2008-12-31 成都理工大学 Method of preparing spherical nanometer SiO2 using powder quartz by chemical precipitation method
CN115448317B (en) * 2022-10-18 2023-10-20 江苏联瑞新材料股份有限公司 Method for simultaneously preparing nano and submicron spherical oxide filler

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