CN101891209A - Method for preparing nano powder of spherical silicon dioxide - Google Patents
Method for preparing nano powder of spherical silicon dioxide Download PDFInfo
- Publication number
- CN101891209A CN101891209A CN 201010232224 CN201010232224A CN101891209A CN 101891209 A CN101891209 A CN 101891209A CN 201010232224 CN201010232224 CN 201010232224 CN 201010232224 A CN201010232224 A CN 201010232224A CN 101891209 A CN101891209 A CN 101891209A
- Authority
- CN
- China
- Prior art keywords
- nano
- powder
- citric acid
- preparation
- ammoniacal liquor
- 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
Images
Abstract
The invention discloses a method for preparing nano powder of spherical silicon dioxide. The method comprises the following steps of: preparing a precursor by using citric acid, tetraethoxysilane and glycol as raw materials and ammonia water as a pH value regulator, and by performing water bath, drying and calcining of the precursor to obtain the nano powder of spherical silicon dioxide, wherein the grain size of the prepared nano powder of spherical silicon dioxide is 20 to 100nm. The method has the advantages of short preparation period, high purity, high yield, simple process equipment and low cost.
Description
Technical field
The invention belongs to technical field of nano material, relate to a kind of preparation method of preparing spherical SiO 2 nano-powder.
Background technology
Nano silica powder is a kind of Performances of Novel Nano-Porous meter level amorphous solid material, is a kind of nontoxic, tasteless, free of contamination ceramic, at aspects such as construction industry, chemical industry, space flight and aviation industry, agriculturals important use is arranged all.Nano silica powder presents unusual characteristic at aspects such as sound, light, electricity, magnetic and thermodynamics, is widely used in aspects such as microelectronics, information material, coating, rubber, plastics, crop seeds treatment agent, rumbling compound, high grade refractory and papermaking.Development nanometer grade silica material is produced high purity, high-tech product is one of current research focus.
The method for preparing at present nano silica powder is a lot, but no matter is vapor phase process, or liquid-phase precipitation method, all has problems such as conversion unit requirement height, complex process, cost height.Additive method also has combustion method, sol-gel method, carburizing reagent method, reverse micelle sol method etc.Methods such as wherein carburizing reagent method, inverse micellar solution method prepare superfine silicon dioxide, and it exists manufacturing process loaded down with trivial details, the not high defective of resultant purity.And the combustion method complex process; The grain diameter that obtains with the precipitator method is big, short texture; With traditional sol-gel method thermal treatment temp height, the Si-OH silanol on the silica sphere is removed by high temperature, and easy reunion of progenitor grows up.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of preparation method of preparing spherical SiO 2 nano-powder, and this method technology is simple, with short production cycle, required equipment is simple, can prepare the spherical nano-silicon dioxide powder of regular shape, good dispersity.
The present invention is achieved through the following technical solutions:
A kind of preparation method of preparing spherical SiO 2 nano-powder may further comprise the steps:
1) citric acid being dissolved in volumetric concentration is that the amount of ammoniacal liquor is as the criterion can dissolve citric acid in 25～28% the ammoniacal liquor, and then according to tetraethoxy: the mol ratio of citric acid=1: 1～1.5 adds tetraethoxy, stirs to make the tetraethoxy dissolving; Add dehydrated alcohol and ethylene glycol more successively, the dehydrated alcohol consumption is 1/3～1/2 of an ammoniacal liquor volume, and the mol ratio of ethylene glycol and citric acid is 1: 1.5～2, is heated to 50～60 ℃ of stirrings it is dissolved fully; Behind ammoniacal liquor accent pH value to 7.0～8.0,80～90 ℃ of water-baths evaporations are until obtaining wet gel;
2) wet gel is carried out the drying foaming under 130～140 ℃ of conditions and obtain xerogel;
3) xerogel is carried out calcining at constant temperature at 600～850 ℃, take out behind calcining 3～5h, obtain nano silica powder.
Described wet gel carries out the drying foaming under air atmosphere.
Described xerogel carries out calcining at constant temperature under air atmosphere.
Described nano silica powder is a kind of preparing spherical SiO 2 nano-powder, and its granular size is 20～100nm.
Compared with prior art, the present invention has following beneficial technical effects:
The preparation method of a kind of preparing spherical SiO 2 nano-powder provided by the invention, because tetraethoxy will all be converted into silicon-dioxide, in this preparation process, do not introduce impurity such as chlorion, need not the suction filtration cleaning, can shorten preparation cycle to remove impurity; And ammoniacal liquor, organic substance citric acid and polyoxyethylene glycol bring into play by water-bath and remove, and all the other remain in and can be carbonized in the calcination process and remove the purity height of prepared nano silica powder, good dispersity.
The preparation method of preparing spherical SiO 2 nano-powder provided by the invention, it is simple also to have production technique, easy to operate, and preparation cycle is short, and productive rate is higher, and facility investment is few, the advantage that cost is low.
Description of drawings
Fig. 1 is the SEM photo figure as a result of spherical nano-silicon dioxide powder.
Embodiment
Embodiment 1
The preparation method of preparing spherical SiO 2 nano-powder may further comprise the steps:
1) citric acid 192.14g (1mol) being dissolved in volumetric concentration is in 25% the 200ml ammoniacal liquor, then according to tetraethoxy: the mol ratio of citric acid=1: 1 adds tetraethoxy, stirs and makes the tetraethoxy dissolving; Add the dehydrated alcohol of 100ml and the ethylene glycol of 0.5mol more successively, be heated to 50 ℃ of stirrings it is dissolved fully; With being made into precursor behind the ammoniacal liquor accent pH value to 7.0, evaporate until the wet gel that obtains white 80 ℃ of water-baths;
2) wet gel is carried out the drying foaming in 130 ℃ stove, under the air atmosphere condition, obtain xerogel;
3) xerogel is carried out calcining at constant temperature putting into kiln under 600 ℃, air atmosphere condition, take out the spherical nano-silicon dioxide powder that obtains loosening behind the calcining 5h.
The SEM photo of gained preparing spherical SiO 2 powder as shown in Figure 1, the gained silicon-dioxide powdery is complete spherical, good dispersity, even particle size distribution, granular size is about 20～50nm.
Embodiment 2
The preparation method of preparing spherical SiO 2 nano-powder may further comprise the steps:
1) citric acid 192.14g (1mol) being dissolved in volumetric concentration is in 25% the 200ml ammoniacal liquor, then according to tetraethoxy: the mol ratio of citric acid=1: 2 adds tetraethoxy, stirs and makes the tetraethoxy dissolving; The dehydrated alcohol and the 0.67mol ethylene glycol that add 66ml more successively are heated to 60 ℃ of stirrings it are dissolved fully; With being made into precursor behind the ammoniacal liquor accent pH value to 8.0, evaporate until the wet gel that obtains white 90 ℃ of water-baths;
2) wet gel is carried out the drying foaming in 140 ℃ stove, under the air atmosphere condition, obtain xerogel;
3) xerogel is carried out calcining at constant temperature putting into kiln under 750 ℃, air atmosphere condition, take out behind the calcining 5h, the spherical nano-silicon dioxide powder that obtains loosening, its granular size is 50～100nm.
Embodiment 3
The preparation method of preparing spherical SiO 2 nano-powder may further comprise the steps:
1) citric acid 192.14g (1mol) being dissolved in volumetric concentration is in 28% the 200ml ammoniacal liquor, then according to tetraethoxy: the mol ratio of citric acid=1: 1.2 adds tetraethoxy, stirs and makes the tetraethoxy dissolving; Add 80ml dehydrated alcohol and 0.6mol ethylene glycol more successively, be heated to 55 ℃ of stirrings it is dissolved fully; With being made into precursor behind the ammoniacal liquor accent pH value to 8.0, evaporate until the wet gel that obtains white 85 ℃ of water-baths;
2) wet gel is carried out the drying foaming in 145 ℃ stove, under the air atmosphere condition, obtain xerogel;
3) xerogel is carried out calcining at constant temperature putting into kiln under 700 ℃, air atmosphere condition, take out behind the calcining 4h, the spherical nano-silicon dioxide powder that obtains loosening, its granular size is 50～100nm.
Embodiment 4
The preparation method of preparing spherical SiO 2 nano-powder may further comprise the steps:
1) citric acid 192.14g (1mol) being dissolved in volumetric concentration is in 28% the 200ml ammoniacal liquor, then according to tetraethoxy: the mol ratio of citric acid=1: 1.8 adds tetraethoxy, stirs and makes the tetraethoxy dissolving; Add 90ml dehydrated alcohol and 0.6mol ethylene glycol more successively, be heated to 58 ℃ of stirrings it is dissolved fully; With being made into precursor behind the ammoniacal liquor accent pH value to 7.5, evaporate until the wet gel that obtains white 83 ℃ of water-baths;
2) wet gel is carried out the drying foaming in 138 ℃ stove, under the air atmosphere condition, obtain xerogel;
3) xerogel is carried out calcining at constant temperature putting into kiln under 650 ℃, air atmosphere condition, take out behind the calcining 2.5h, the spherical nano-silicon dioxide powder that obtains loosening, its granular size is 20～100nm.
Embodiment 5
The preparation method of preparing spherical SiO 2 nano-powder may further comprise the steps:
1) citric acid 192.14g (1mol) being dissolved in volumetric concentration is in 25% the 200ml ammoniacal liquor, then according to tetraethoxy: the mol ratio of citric acid=1: 1.6 adds tetraethoxy, stirs and makes the tetraethoxy dissolving; Add 100ml dehydrated alcohol and 0.55mol ethylene glycol more successively, be heated to 58 ℃ of stirrings it is dissolved fully; With being made into precursor behind the ammoniacal liquor accent pH value to 7.2, evaporate until the wet gel that obtains white 90 ℃ of water-baths;
2) wet gel is carried out the drying foaming in 136 ℃ stove, under the air atmosphere condition, obtain xerogel;
3) xerogel is carried out calcining at constant temperature putting into kiln under 720 ℃, air atmosphere condition, take out behind the calcining 3h, the spherical nano-silicon dioxide powder that obtains loosening, its granular size is 20～80nm.
Claims (4)
1. the preparation method of a preparing spherical SiO 2 nano-powder is characterized in that, may further comprise the steps:
1) citric acid being dissolved in volumetric concentration is that the amount of ammoniacal liquor is as the criterion can dissolve citric acid in 25～28% the ammoniacal liquor, and then according to tetraethoxy: the mol ratio of citric acid=1: 1～1.5 adds tetraethoxy, stirs to make the tetraethoxy dissolving; Add dehydrated alcohol and ethylene glycol more successively, the dehydrated alcohol consumption is 1/3～1/2 of an ammoniacal liquor volume, and the mol ratio of ethylene glycol and citric acid is 1: 1.5～2, is heated to 50～60 ℃ of stirrings it is dissolved fully; Behind ammoniacal liquor accent pH value to 7.0～8.0,80～90 ℃ of water-baths evaporations are until obtaining wet gel;
2) wet gel is carried out the drying foaming under 130～140 ℃ of conditions and obtain xerogel;
3) xerogel is carried out calcining at constant temperature at 600～850 ℃, take out behind calcining 3～5h, obtain nano silica powder.
2. the preparation method of preparing spherical SiO 2 nano-powder as claimed in claim 1 is characterized in that, described wet gel carries out the drying foaming under air atmosphere.
3. the preparation method of preparing spherical SiO 2 nano-powder as claimed in claim 1 is characterized in that, described xerogel carries out calcining at constant temperature under air atmosphere.
4. the preparation method of preparing spherical SiO 2 nano-powder as claimed in claim 1 is characterized in that, described nano silica powder is the preparing spherical SiO 2 nano-powder, and its granular size is 20～100nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102322247A CN101891209B (en) | 2010-07-21 | 2010-07-21 | Method for preparing nano powder of spherical silicon dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102322247A CN101891209B (en) | 2010-07-21 | 2010-07-21 | Method for preparing nano powder of spherical silicon dioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101891209A true CN101891209A (en) | 2010-11-24 |
| CN101891209B CN101891209B (en) | 2012-05-09 |
Family
ID=43100587
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010102322247A Active CN101891209B (en) | 2010-07-21 | 2010-07-21 | Method for preparing nano powder of spherical silicon dioxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101891209B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432193A (en) * | 2011-08-23 | 2012-05-02 | 陕西科技大学 | Preparation method of organic electrochromic composite membrane |
| CN104229807A (en) * | 2014-09-11 | 2014-12-24 | 天津市风船化学试剂科技有限公司 | Method for preparing high-purity silica |
| CN104445220A (en) * | 2014-11-28 | 2015-03-25 | 新沂市天悦石英有限公司 | Method for preparing nano nanosilicon dioxide powder by vinyl triethoxyl silane |
| CN104909377A (en) * | 2015-06-12 | 2015-09-16 | 湖南尔康制药股份有限公司 | Preparation method of nano silicon dioxide |
| CN105967723A (en) * | 2016-05-05 | 2016-09-28 | 陕西科技大学 | Preparation method of silica porous material |
| CN110479954A (en) * | 2019-08-19 | 2019-11-22 | 安徽省含山县兴建铸造厂 | A kind of model casting precision casting shell fire resistant covering material |
| CN111960427A (en) * | 2020-08-31 | 2020-11-20 | 浙江华飞电子基材有限公司 | Preparation method and device of nano spherical silicon dioxide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591535A (en) * | 2009-06-29 | 2009-12-02 | 彩虹集团公司 | A kind of preparation method of alkaline-earth silicate fluorescent powder of activated by rare earth elements |
-
2010
- 2010-07-21 CN CN2010102322247A patent/CN101891209B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591535A (en) * | 2009-06-29 | 2009-12-02 | 彩虹集团公司 | A kind of preparation method of alkaline-earth silicate fluorescent powder of activated by rare earth elements |
Non-Patent Citations (1)
| Title |
|---|
| 《天津化工》 20050131 郭宇等 溶胶-凝胶法制备纳米二氧化硅 第34-35页 1-4 第19卷, 第1期 2 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432193A (en) * | 2011-08-23 | 2012-05-02 | 陕西科技大学 | Preparation method of organic electrochromic composite membrane |
| CN102432193B (en) * | 2011-08-23 | 2013-07-31 | 陕西科技大学 | Preparation method of organic electrochromic composite membrane |
| CN104229807A (en) * | 2014-09-11 | 2014-12-24 | 天津市风船化学试剂科技有限公司 | Method for preparing high-purity silica |
| CN104445220A (en) * | 2014-11-28 | 2015-03-25 | 新沂市天悦石英有限公司 | Method for preparing nano nanosilicon dioxide powder by vinyl triethoxyl silane |
| CN104445220B (en) * | 2014-11-28 | 2016-08-24 | 新沂市天悦石英有限公司 | A kind of method preparing nano-silica powder with VTES |
| CN104909377A (en) * | 2015-06-12 | 2015-09-16 | 湖南尔康制药股份有限公司 | Preparation method of nano silicon dioxide |
| CN105967723A (en) * | 2016-05-05 | 2016-09-28 | 陕西科技大学 | Preparation method of silica porous material |
| CN110479954A (en) * | 2019-08-19 | 2019-11-22 | 安徽省含山县兴建铸造厂 | A kind of model casting precision casting shell fire resistant covering material |
| CN111960427A (en) * | 2020-08-31 | 2020-11-20 | 浙江华飞电子基材有限公司 | Preparation method and device of nano spherical silicon dioxide |
| CN111960427B (en) * | 2020-08-31 | 2023-09-15 | 浙江华飞电子基材有限公司 | Preparation method and device of nano spherical silicon dioxide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101891209B (en) | 2012-05-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101891209B (en) | Method for preparing nano powder of spherical silicon dioxide | |
| CN101891206B (en) | Preparation method of SiO2/TiO2 composite microspheres | |
| CN102701288B (en) | Perovskite composite oxide LaFeO3 monodisperse micrometer hollow balls and preparation method thereof | |
| CN101891210B (en) | Preparation method of nano silicon dioxide powder | |
| CN102241516B (en) | Method for preparing Li4SiO4 ceramic powder by water-based sol-gel process | |
| CN101585544B (en) | Method for preparing aluminum borate nanowire | |
| CN101891207B (en) | Method for preparing SiO2/TiO2 composite powder | |
| CN102148351A (en) | Preparation method for electrode material of lithium battery | |
| CN102503387B (en) | Method for preparing high-purity super-fine mullite powder | |
| CN110407192A (en) | Three-dimensional order graded porous carbon photonic crystal method is prepared using metal organic frame | |
| CN109468684B (en) | Preparation method of yttrium oxide nano-beam whisker | |
| CN102874823A (en) | Method for preparing silicon dioxide hollow microspheres with uniform shape by taking pollen grains as biological template | |
| CN103641122A (en) | Preparation method for multilevel mesoporous silica nanoparticles | |
| CN101891974B (en) | Method for preparing TiO2/SiO2 composite powder | |
| CN104107689A (en) | Macroporous nanocomposite and preparation method thereof | |
| CN109111230A (en) | A kind of yttrium oxide-bitter earth nano composite granule and preparation method thereof | |
| CN101891208A (en) | Method for preparing submicron silicon dioxide spherical particles | |
| CN101665237B (en) | Preparation method of spherical aluminum-doped zinc oxide nanometer powder | |
| CN107792888A (en) | A kind of high-specific surface area ZnCo2O4Preparation method | |
| CN105731518B (en) | Normal-temperature crystallization preparation method of octahedron cuprous oxide crystal | |
| CN105980333B (en) | The manufacturing method of forsterite particle | |
| CN101279766A (en) | Preparation of spherical nano-titanic oxide | |
| CN101456561A (en) | Method for preparing nano mullite powder | |
| CN103833080B (en) | A kind of preparation method of molybdic acid cadmium porous ball | |
| CN105036148B (en) | Preparation method for flowerlike Li2Si2O5 powder |
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 | ||
| ASS | Succession or assignment of patent right |
Owner name: ZHEJIANG HUAFEI ELECTRONIC BASE MATERIAL CO., LTD. Free format text: FORMER OWNER: SHAANXI UNIVERSITY OF SCIENCE AND TECHNOLOGY Effective date: 20140106 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 710021 XI AN, SHAANXI PROVINCE TO: 313000 HUZHOU, ZHEJIANG PROVINCE |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20140106 Address after: 313000, Wuxing District, Zhejiang province Huzhou Yang Port Industrial Zone Patentee after: ZHEJIANG HUAFEI ELECTRONIC BASE MATERIAL CO., LTD. Address before: 710021 Shaanxi province Xi'an Weiyang University Park No. 1 Patentee before: Shaanxi University of Science and Technology |