CN1407026A - Micro-size silica powder preparation - Google Patents
Micro-size silica powder preparation Download PDFInfo
- Publication number
- CN1407026A CN1407026A CN 02118210 CN02118210A CN1407026A CN 1407026 A CN1407026 A CN 1407026A CN 02118210 CN02118210 CN 02118210 CN 02118210 A CN02118210 A CN 02118210A CN 1407026 A CN1407026 A CN 1407026A
- Authority
- CN
- China
- Prior art keywords
- micro
- silicon
- silica powder
- silicon sol
- size silica
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Silicon Compounds (AREA)
Abstract
A process for preparing superfine SiO2 powder from silicon sol includes such steps as choosing proper raw silicon sol, gelatinizing and drying. Its advantages are controllable granularity (5-100 nm), high purity and size uniformity, and low cost.
Description
Technical field
The present invention relates to a kind of production method of micro-size silica powder, more particularly, is a kind of method that is prepared micro-size silica powder by silicon sol.
Background technology
Superfine silicon dioxide is a kind of submicron or nano level silicon-dioxide powdery, and its primary partical size is below 1um, and generally at 5-100nm, minimum can be controlled in the 5nm-20nm scope.Silanol base and residual oxygen base are rich in its surface, and its performance is different from general trickle silicon-dioxide powdery, can be widely used in the industries such as coating, resin, plastics, electronics, pottery.
The present method of making micro-size silica powder has a variety of, relatively is typically tetraethyl silicate (ETOS) sol-gel method.Patent as applications such as the Zhang Lide of solid-state physics institute of the disclosed Chinese Academy of Sciences in 1996 of Patent Office of the People's Republic of China, publication number is: 1117022A, " a kind of preparation method of silicon dioxide powder with controllable nanon size ", it is raw material that this patent adopts ETOS, by hydrolysis generate silica dioxide gel again the drying pyroprocessing make the nano level superfine silicon-dioxide powdery.Its shortcoming is that the raw silicon acetoacetic ester that adopted costs an arm and a leg and causes the products made thereby cost higher.
And adopt silicon sol is the patent US5352645 (1994) that U.S. E.I.du Pont deNemours and Company is arranged " Silica microspheres; method of improving attrition resistance and use (the silicon dioxide microsphere body improves the methods and applications of wear resistance) " of raw material production superfine silicon dioxide.It is raw material that this patent adopts silicon sol, adds additive such as ammonium citrate or urea etc., by spraying drying, method for calcinating, can prepare the high spraying silicon dioxide microsphere of abrasion resistance.Its shortcoming is the particle diameter of the particle diameter of the silicon-dioxide powdery that makes the in this way little drop of silicon sol during corresponding to spraying, and its diameter is 1um-5um, and can not reach the requirement of nano level product near the particle diameter of silicon sol micelle.
Adopting silicate in addition is that raw material is produced superfine silicon dioxide by methods such as chemical precipitation method, carburizing reagent method, inverse micellar solution methods, but these methods all exist manufacturing process loaded down with trivial details, the not high defective of resultant purity.
Summary of the invention
The objective of the invention is to, overcome existing preparation technology's deficiency, adopt cost of material lower, the simple method of production technique can obtain the silicon-dioxide powdery close with the silicon sol particle size analysis, and particle diameter is even, purity is high, be easy to large-scale production.
It is raw material that the present invention adopts silicon sol, directly makes micro-size silica powder by gelling, drying.
The advantage that adopts the inventive method to prepare micro-size silica powder is: the one, and cost of material is cheap, greatly reduces production cost of products, and the silicon sol price is about 1/5th of tetraethyl silicate price on year-on-year basis; The 2nd, the product purity height, and can be according to raw silicon colloidal sol size control micro-size silica powder diameter, superfine silicon dioxide narrow diameter distribution; The 3rd, present method is easy to large-scale production.
Embodiment
Embodiment one:
Select commercial silicon sol for use, reach the AS-25 of chemical industry company limited silicon sol as Shangyu, Zhejiang Province city space, this silicon sol dioxide-containing silica is 25 ± 1%, and particle size analysis is 5-20nm, and its product purity is higher.
Getting particle diameter is 8nm left and right sides silicon sol 50g, under agitation condition, slowly drip 95% ethanol, make progressively dehydrating gel of silicon sol micelle, to abundant gel,, remove major part and contain aqueous ethanolic solution through natural subsidence or filter method, obtain transparent wet gel, put into 200 ℃ of baking oven bakings 6 hours, treat can obtain the about 12g of lily micro-size silica powder behind the naturally cooling, its diameter of particle size is about 9nm.Embodiment two:
Getting particle diameter is 8nm left and right sides AS-25 silicon sol 50g, under agitation condition, slowly drip methyl alcohol, make progressively dehydrating gel of silicon sol, to abundant gel, remove major part earlier through natural subsidence or filter method and contain methanol aqueous solution, again wet gel is put into 200 ℃ of baking oven bakings 6 hours, treat can obtain the about 12g of lily micro-size silica powder behind the naturally cooling, its diameter of particle size is about 9nm.
In addition, be to improve the purity of superfine silicon dioxide, after wet gel is put into the baking oven baking again the oven dry thing 800 ℃-1000 ℃ calcinings 1-3 hour, to remove remaining moisture content and other impurity, treat can obtain behind the naturally cooling micro-size silica powder of high purity white
Certainly,,, can select the silicon sol of different colloidal particle sizes for use, and ethanol or methyl alcohol after filtering are all recyclable according to the particle diameter requirement of required silicon-dioxide powdery according to the method for embodiment one or embodiment two.
The method technology that the present invention produces micro-size silica powder is simple, process is easy to control, can select for use the chemical industry conventional equipment can realize large-scale commercial production, and the primary particle diameter of its silicon-dioxide powdery is close with the silicon sol particle diameter, the silicon-dioxide powdery purity height that makes, particle diameter is even.
Claims (4)
1, a kind of preparation method of superfine silicon dioxide, it is a raw material with the silicon sol, it is characterized in that its technology directly makes micro-size silica powder by gelling, drying.
2, the preparation method of superfine silicon dioxide according to claim 1 is characterized in that the gelling operation has adopted jelling agent, and described jelling agent is the dewatering agent of silicon sol gentleness.
3, the preparation method of superfine silicon dioxide according to claim 2 is characterized in that described jelling agent is an ethanol.
4, the preparation method of superfine silicon dioxide according to claim 2 is characterized in that described jelling agent is a methyl alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02118210 CN1215127C (en) | 2001-08-19 | 2002-04-25 | Micro-size silica powder preparation |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN01125360.6 | 2001-08-19 | ||
| CN01125360 | 2001-08-19 | ||
| CN 02118210 CN1215127C (en) | 2001-08-19 | 2002-04-25 | Micro-size silica powder preparation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1407026A true CN1407026A (en) | 2003-04-02 |
| CN1215127C CN1215127C (en) | 2005-08-17 |
Family
ID=25740467
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02118210 Expired - Fee Related CN1215127C (en) | 2001-08-19 | 2002-04-25 | Micro-size silica powder preparation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1215127C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1330714C (en) * | 2005-01-18 | 2007-08-08 | 武汉理工大学 | Method of preparing nano-silicone dioxide capable of inducing poly vinyl chloide crystallization |
| CN1789185B (en) * | 2004-12-15 | 2010-06-09 | 广东工业大学 | Method for preparing ultrafined glass state powder |
| CN101225249B (en) * | 2007-12-07 | 2010-11-17 | 东华大学 | Method for preparing lipophilic nano SiO2 powder |
| CN102618926A (en) * | 2011-01-31 | 2012-08-01 | 姜兴盛 | Traditional Chinese medicine for treating tonsillitis and pharyngitis |
-
2002
- 2002-04-25 CN CN 02118210 patent/CN1215127C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1789185B (en) * | 2004-12-15 | 2010-06-09 | 广东工业大学 | Method for preparing ultrafined glass state powder |
| CN1330714C (en) * | 2005-01-18 | 2007-08-08 | 武汉理工大学 | Method of preparing nano-silicone dioxide capable of inducing poly vinyl chloide crystallization |
| CN101225249B (en) * | 2007-12-07 | 2010-11-17 | 东华大学 | Method for preparing lipophilic nano SiO2 powder |
| CN102618926A (en) * | 2011-01-31 | 2012-08-01 | 姜兴盛 | Traditional Chinese medicine for treating tonsillitis and pharyngitis |
| CN102618926B (en) * | 2011-01-31 | 2015-04-15 | 姜兴茂 | Method for preparing spherical nanomonocrystalline particle |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1215127C (en) | 2005-08-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5868520B2 (en) | Method for producing precipitated silica | |
| CN102897779B (en) | Preparation method of transparent silicon dioxide aerogel | |
| JPWO2012096172A1 (en) | Method for producing particles containing metal oxide and method for producing aggregates of metal oxide colloidal particles | |
| TW201641544A (en) | Aerogel granule and preparation method thereof | |
| JP2004315300A (en) | Silica fine particle, silica colloid in which silica fine particles are dispersed and method of manufacturing the same | |
| CN102757085A (en) | Process for preparing nanometer zinc oxide with sol-gel process | |
| CN101346304A (en) | Methods for production of metal oxide nano particles with controlled properties, and nano particles and preparationsproduced thereby | |
| KR20080093772A (en) | Method for preparing permanently hydrophobic aerogel powder having increased particle size and density and aerogel powder therefrom | |
| CN100542955C (en) | A kind of preparation method of nano silicon dioxide | |
| CN101891209B (en) | Method for preparing nano powder of spherical silicon dioxide | |
| CN1215127C (en) | Micro-size silica powder preparation | |
| CN111422877A (en) | Preparation method and surface modification method of nano silicon dioxide | |
| Gao et al. | Nanoscale silicon dioxide prepared by sol-gel process | |
| CN1830775A (en) | Method of preparing spherical nanometer SiO2 using powder quartz by chemical precipitation method | |
| CN105060306A (en) | Preparation method of silica nanotube | |
| CN110980737A (en) | Modification method for silanization of surface of silicon carbide micro powder and modified silicon carbide micro powder | |
| CN114195158A (en) | Preparation method of high-purity monodisperse nano spherical silicon dioxide powder | |
| CN105980333B (en) | The manufacturing method of forsterite particle | |
| CN101774594A (en) | Method for preparing modified acicular wollastonite | |
| CN113104877A (en) | Preparation method and application of superfine dolomite | |
| CN1291991C (en) | Preparation method of multihydroxy sesqui siloxane | |
| Bugrov et al. | Distribution of zirconia nanoparticles in the matrix of poly (4, 4′-oxydiphenylenepyromellitimide) | |
| CN1704452A (en) | Process for preparing nano silicon dioxide particles | |
| CN1830774A (en) | Method of preparing high purity spherical nanometer noncrystalline silicon micropowder using natural powder quartz | |
| Vero et al. | Homogeneous self-cleaning coatings on cellulose materials derived from TIP/TiO 2 P25 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Zhejiang Xinli Chemicals Co., Ltd. Assignor: Zhang Haolong Contract fulfillment period: 2008.10.24 to 2014.10.23 contract change Contract record no.: 2008330002061 Denomination of invention: Micro-size silica powder preparation Granted publication date: 20050817 License type: Exclusive license Record date: 20081117 |
|
| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.10.24 TO 2014.10.23; CHANGE OF CONTRACT Name of requester: ZHEJIANG PROVINCE XINLI CHEMICAL CO., LTD. Effective date: 20081117 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20050817 Termination date: 20150425 |
|
| EXPY | Termination of patent right or utility model |