CN1089077C - Surficial modification process for SiO2 sol particles - Google Patents
Surficial modification process for SiO2 sol particles Download PDFInfo
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- CN1089077C CN1089077C CN98124657A CN98124657A CN1089077C CN 1089077 C CN1089077 C CN 1089077C CN 98124657 A CN98124657 A CN 98124657A CN 98124657 A CN98124657 A CN 98124657A CN 1089077 C CN1089077 C CN 1089077C
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- sio
- colloidal sol
- solution
- surficial
- sol
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Abstract
The present invention relates to a surface modification method of SiO2 sol particles. In the method, a sol-gel method is used for modifying the surfaces of the SiO2 sol particles through organic macromolecules for directly preparing SiO2 sol with different spatial conformations; necessary conditions are prepared for regulating and controlling the material pore canal properties and improving the surface properties. The method of the present has the advantages of simple technology and convenient operation.
Description
The invention belongs to colloidal sol grain modifying method, relate in particular to a kind of SiO
2The colloidal sol surface modification method.
The develop rapidly of modern science and technology has brought many new opportunities to develop for the material field, from performance and requirement, on the nanometer level implementation structure controlled be the research tendency of nanometer synthetic technology in recent years.Utilize organic macromolecule in solution, to have a conformation, by to SiO
2The finishing of colloidal sol nano colloidal particles, and then modulation colloidal sol network structure is the prerequisite of the controlled nano material synthetic technology of implementation structure.Report SiO at present
2Preparation of nanomaterials is a lot, but relates to controlled to powder structure mostly, and about to SiO
2The report of colloidal sol network structure regulation and control is then considerably less.Chinese invention patent 1145331 relates under the modulation of tensio-active agent, and a kind of controllable grain size non-crystal nm SiO is provided
2Technology of preparing; Collosol structure is not studied, 1150124 modification techniques of having reported a kind of colloidal sol surface of Chinese invention patent is characterized in that can preparing the metal-ceramic composite membrane by the modified metal active constituent.As seen aforesaid method only relates to modification and the technology of preparing to powder, does not almost relate to SiO
2The regulation and control of colloidal sol network structure.
But the purpose of this invention is to provide a kind of modulation SiO
2The colloidal sol surface modification method of molten chamber network structure.
The present invention adopts sol-gel method to modify SiO by organic macromolecule
2The colloidal sol surface directly prepares the SiO with different spaces conformation
2The colloidal sol network structure.
The present invention includes following steps:
1. add tetraethoxy in half of the total consumption of ethanolic soln, the back that stirs forms solution (I);
2. quantitative water, ammoniacal liquor and additive are added in second half of the total consumption of ethanolic soln, mix the back and form solution (II);
3. in whipping process, solution (II) is slowly added in the solution (I), continue to stir 30 minutes, then mixed solution is changed in the molten device of close valve of tetrafluoroethylene over to constant temperature ageing, the SiO that promptly obtains having different spaces conformation network structure
2Colloidal sol;
The proportioning (mol ratio) that it is characterized in that colloidal sol is as follows:
Ethanol: water: additive: ammoniacal liquor: tetraethoxy=
(10-100)∶(0.5-10)∶(0.01-0.1)∶(1.0×10
-5)∶1；
20-260 ℃ of aforesaid ageing temperature, digestion time 0.5 day-1 year.
Aforesaid additive can be polyoxyethylene glycol (PEG), fatty alcohol-polyoxyethylene ether (AEO), aliphatic alcohol polyethenoxy polyoxypropylene ether copolymer (PEO-PPO-PEO).
Compared with the prior art the present invention has following advantage:
Present method technology is simple, and is easy to operate, and raw material is easy to get, and adopts single stage method can prepare the SiO with various space conformations
2Colloidal sol adds the SiO that polyoxyethylene glycol (PEC) obtains
2Colloidal sol has the cyclic network structure, adds the SiO that fatty alcohol-polyoxyethylene ether (AEO) obtains
2Colloidal sol has bar-shaped network structure, adds the SiO that aliphatic alcohol polyethenoxy polyoxypropylene ether copolymer (PEO-PPO-PEO) obtains
2Colloidal sol has dendritic network structure.Be next step regulation and control SiO
2Nano material pore properties and improve surface properties and prepared prerequisite.
Embodiment 1
The 20ml tetraethoxy is dissolved in the dehydrated alcohol of 100ml and stirs 15min; With 3.2ml H
2O, 110ml dehydrated alcohol, 0.1ml6MNH
3H
2O and the abundant mixing of 0.1ml PEG200.With above-mentioned two kinds of colloidal sol mixings, 20 ℃ of following ageings 150 days or 60 ℃ of following ageings 20 days, promptly prepare SiO in the encloses container of the tetrafluoroethylene of packing into then with loop network structure
2Colloidal sol.
Embodiment 2
In the foregoing description 1, also can add 5mlPEG200 or PEG600, under the same conditions, prepare SiO with loop network structure
2Colloidal sol.
Embodiment 3
In the foregoing description 1, also can add 10mlPEG200 or PEG600, under the same conditions, prepare SiO with loop network structure
2Colloidal sol.
Embodiment 4
In the foregoing description 1, also can add the 0.1ml polymerization degree and be 3 the AEO or the polymerization degree and be 15 AEO, under the same conditions, prepare SiO with bar-shaped network structure
2Colloidal sol.
Embodiment 5
In the foregoing description 1, also can add the 5ml polymerization degree and be 3 the AEO or the polymerization degree and be 15 AEO, under the same conditions, prepare SiO with bar-shaped network structure
2Colloidal sol.
Embodiment 6
In the foregoing description 1, also can add the 10ml polymerization degree and be 3 the AEO or the polymerization degree and be 15 AEO, under the same conditions, prepare SiO with bar-shaped network structure
2Colloidal sol.
Embodiment 7
In the foregoing description 1, also can add 0.1ml multipolymer (PEO)
3-(PPO)
30-(PEO)
3Or multipolymer (PEO)
4-(PPO)
39-(PEO)
4, under the same conditions, prepare SiO with dendroid network structure
2Colloidal sol.
Embodiment 8
In the foregoing description 1, also can add 5ml multipolymer (PEO)
3-(PPO)
30-(PEO)
3Or multipolymer (PEO)
4-(PPO)
89-(PEO)
4, under the same conditions, prepare SiO with dendroid network structure
2Colloidal sol.
Embodiment 9
In the foregoing description 1, also can add 10ml multipolymer (PEO)
3-(PPO)
30-(PEO)
3Or multipolymer (PEO)
4-(PPO)
39-(PEO)
4, under the same conditions, prepare SiO with dendroid network structure
2Colloidal sol.
Claims (2)
1. a surficial modification process for SiO 2 sol particles comprises the steps:
(1) add tetraethoxy in half of the total consumption of ethanolic soln, the back that stirs forms solution (I);
(2) quantitative water, ammoniacal liquor and additive are added in second half of the total consumption of ethanolic soln, mix the back and form solution (II);
(3) in whipping process, solution (II) is slowly added in the solution (I), continue to stir 30 minutes, then mixed solution is changed in the encloses container of tetrafluoroethylene, under 20-260 ℃ of ageing temperature, ageing 0.5 day-1 year, the SiO that promptly obtains having different spaces conformation network structure
2Colloidal sol;
The proportioning (mol ratio) that it is characterized in that colloidal sol is as follows:
Ethanol: water: additive: ammoniacal liquor: tetraethoxy=
(10-100)∶(0.5-10)∶(0.01-0.1)∶1.0×10
-5∶1。
2. a kind of surficial modification process for SiO 2 sol particles according to claim 1 is characterized in that described additive is polyoxyethylene glycol, Fatty Alcohol(C12-C14 and C12-C18) oxygen Vinyl Ether, aliphatic alcohol polyethenoxy polyoxypropylene ether copolymer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98124657A CN1089077C (en) | 1998-11-04 | 1998-11-04 | Surficial modification process for SiO2 sol particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98124657A CN1089077C (en) | 1998-11-04 | 1998-11-04 | Surficial modification process for SiO2 sol particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1253117A CN1253117A (en) | 2000-05-17 |
| CN1089077C true CN1089077C (en) | 2002-08-14 |
Family
ID=5228740
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98124657A Expired - Fee Related CN1089077C (en) | 1998-11-04 | 1998-11-04 | Surficial modification process for SiO2 sol particles |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1089077C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807224B (en) * | 2011-06-05 | 2014-10-01 | 广州纳科米兹新材料有限公司 | Application of silica material with disordered microporous structure and long-chain alkyl groups |
| CN102807225B (en) * | 2011-06-05 | 2015-07-29 | 广州纳科米兹新材料有限公司 | Preparation and the fatty alcohol-polyoxyethylene ether of unordered porous silica silicon materials are applied in this preparation |
| CN103359954A (en) * | 2012-04-01 | 2013-10-23 | 比亚迪股份有限公司 | Preparation method of silicon dioxide super-hydrophobic thin film and super-hydrophobic material |
| CN103991876B (en) * | 2014-05-06 | 2016-11-02 | 上海大学 | Organically-modified silicon dioxide gel and preparation method thereof |
| CN106832417B (en) * | 2017-03-14 | 2019-01-18 | 北京化工大学 | Use aliphatic APEO modified white carbon black and its method compound with rubber |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045754A (en) * | 1989-03-21 | 1990-10-03 | 卡伯特公司 | The hydration aqueous colloidal dispersion that contains the fuming silicon-dioxide of acid and stablizer |
| CN1150124A (en) * | 1995-11-14 | 1997-05-21 | 中国科学院大连化学物理研究所 | Method for in-situ dressing surface of sol particles |
| CN1155514A (en) * | 1996-01-25 | 1997-07-30 | 天津市化学试剂一厂 | Manufacture of high purity, high concentration and high granularity large granular silicon dioxide gel |
-
1998
- 1998-11-04 CN CN98124657A patent/CN1089077C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045754A (en) * | 1989-03-21 | 1990-10-03 | 卡伯特公司 | The hydration aqueous colloidal dispersion that contains the fuming silicon-dioxide of acid and stablizer |
| CN1150124A (en) * | 1995-11-14 | 1997-05-21 | 中国科学院大连化学物理研究所 | Method for in-situ dressing surface of sol particles |
| CN1155514A (en) * | 1996-01-25 | 1997-07-30 | 天津市化学试剂一厂 | Manufacture of high purity, high concentration and high granularity large granular silicon dioxide gel |
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| Publication number | Publication date |
|---|---|
| CN1253117A (en) | 2000-05-17 |
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| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
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Granted publication date: 20020814 Termination date: 20111104 |