CN1757681A - Nanometer SiO2 powder dispersion method - Google Patents
Nanometer SiO2 powder dispersion method Download PDFInfo
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- CN1757681A CN1757681A CN 200510012946 CN200510012946A CN1757681A CN 1757681 A CN1757681 A CN 1757681A CN 200510012946 CN200510012946 CN 200510012946 CN 200510012946 A CN200510012946 A CN 200510012946A CN 1757681 A CN1757681 A CN 1757681A
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- Prior art keywords
- nanometer sio
- powder
- reaction
- dodecylbenzene sulfonate
- sodium dodecylbenzene
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Abstract
A process for dispersing SiO2 nano-particles includes such steps as adding nano-class SiO2 sol into reactor, stirring while dripping Al(NO3)3.9H2O, regulating pH=7.5-8.0, reaction to coat Al(OH)3 on the surface of SiO2 nano-particle, washing with de-ionized water, drying, dissolving sodium dodecylphenylsulfonate in de-ionized water, adding said coated SiO2 nano-particles, regulating pH=6, and stirring while reacting to obtain Al(OH)3 coated and sodium dodecylphenylsulfonate modified SiO2 nano-particles. It can be used as the functional filler of plastic, rubber, paint, adhesive, etc.
Description
Technical field
The present invention relates to a kind of dispersing method of nano-powder material, particularly utilize the nanometer SiO of aluminium hydroxide/Sodium dodecylbenzene sulfonate surface coating modification
2The dispersing method of powder body material.
Background technology
Nanometer SiO
2Have higher surface activity and become key tendency, but higher surface activity and become key to be inclined to cause its surface energy very high, very easily reunite between the particle, in order to improve nanometer SiO
2Dispersiveness, the investigator has carried out big quantity research to dispersion agent, the dispersing method that uses.Utilizing acrylic acid derivative as Ou Yuchun etc. is surfactant-modified nanometer SiO
2, joining again in the methyl methacrylate solution that contains superoxide, bulk thermal polymerization obtains nanometer SiO
2Matrix material; Espiard has studied ethyl propenoate at nanometer SiO
2Graft polymerization reaction on the surfactivity point, the nanometer SiO that has obtained to have good dispersion
2Particle; (molar mass is about 10000 to German patent DE 4433542 usefulness polysilanes, by 3-H
2N-C
6H
4The SiPr repeating unit is formed) and the silica powder mixing, under UV-irradiation, stir 5h, obtain nanometer SiO
2Active filler; TeofilTesionouski etc. utilize hydrosulphonyl silane, vinyl silicane coupling agent to nanometer SiO
2After carrying out surface treatment, the nano powder surface hydroxy number reduces in a large number.Japanese Patent JPOS10514 handles nanometer SiO with the silandiol derivative
2, and in the Hybrid Heating process, add catalyzer (HCl or alkali metal hydroxide or amine), the nanometer SiO after the modification
2Functional during as silicone gasket.
Above-mentioned dispersing method exists with strong points, and range of application is narrow, and dispersion agent uses cats product more, costs an arm and a leg, and has deficiencies such as toxicity.For this reason, the present invention proposes inorganic/organic surface coating modification dispersion method, promptly earlier with Al (OH)
3To nanometer SiO
2Particle carries out the surface and coats, and its interface electrical property is changed, the direction skew that iso-electric point increases to the pH value, thus make nanometer SiO
2Powder can carry out under near the neutral condition the absorption of anion surfactant, uses anion surfactant to carry out modification then, realizes nanometer SiO
2Dispersion.
Summary of the invention
The problem to be solved in the present invention is to adopt cats product to nanometer SiO
2When powder body material disperses, cost an arm and a leg, have toxicity.For this reason, the invention provides a kind of cheap and avirulent nanometer SiO
2The dispersing method of powder body material.
The compound dispersing method of the present invention adopts inorganic/organic surface coating modification is to nanometer SiO
2Disperse, at first utilize aluminium hydroxide by precipitin reaction at nanometer SiO
2The surface forms one deck " coating ", changes nanometer SiO
2Particulate interface electrical property adopts Sodium dodecylbenzene sulfonate then, carries out surface modification treatment by chemical reaction, realizes nanometer SiO
2Dispersion.Its concrete processing method follows these steps to carry out successively:
The first step, inorganic coating: in the reactor that has whipping appts and fluid flow tube, adding the 1L solid-to-liquid ratio is the nanometer SiO of 50g/L
2Colloidal sol stirs, and is the Al (NO of 0.02～0.1mol/L again with 20ml concentration
3)
39H
2O splashes into from fluid flow tube, pH value with aqueous solution of urea conditioned reaction liquid, it is remained between 7.5～8.0, under 75 ℃ temperature condition, reaction 2h is after reaction finishes, use deionized water wash, dewater with dehydrated alcohol again, and then under 110 ℃ temperature condition, be dried to constant weight, promptly make the surface and coat Al (OH)
3Nanometer SiO
2Powder;
Second step, organically-modified: with mass percent is that 0.5%～2.0% Sodium dodecylbenzene sulfonate adds and has in the reactor of whipping appts, after adding the dissolving evenly of 1L deionized water and stirring, be the above-mentioned surface coating Al (OH) that makes of proportioning adding of 50g/L by solid-to-liquid ratio
3Nanometer SiO
2Powder, the pH=6 of conditioned reaction liquid, stirring reaction 2h, after reaction finishes, use deionized water wash earlier, dewater with dehydrated alcohol again, under 110 ℃ temperature condition, be dried to constant weight then, promptly make the nanometer SiO that surface of aluminum hydroxide coats the Sodium dodecylbenzene sulfonate surface modification
2Powder.
The present invention is by implementing technique scheme, with existing nanometer SiO
2Powder body material uses cats product that it is carried out the dispersive method usually and compares, earlier with Al (OH)
3To nanometer SiO
2Particle carries out the surface and coats, and its interface electrical property is changed, the direction skew that iso-electric point increases to the pH value, thus make SiO
2Powder can carry out under near the neutral condition the absorption of anion surfactant, has reduced the cost of dispersion agent when making modified condition become gentle, and nontoxicity.Processing method of the present invention is simple, easy to operate, modified effect is good, disperse the back powder to can be used as a kind of functional stuffing, be applied in the product of all conglomeraties such as plastics, rubber, coating, tamanori, with the mechanical property of raising material and the over-all properties of material, it is with strong points to have overcome other dispersing method, the deficiency that range of application is narrow.
Description of drawings
Fig. 1 is without dispersive nanometer SiO of the present invention
2The stereoscan photograph of powder
Fig. 2 is through dispersive nanometer SiO of the present invention
2The stereoscan photograph of powder
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is further detailed
Embodiment 1
The first step, inorganic coating: in the reactor that has whipping appts and fluid flow tube, adding the 1L solid-to-liquid ratio is the nanometer SiO of 50g/L
2Colloidal sol is the Al (NO of 0.03mol/L with 20ml concentration
3)
39H
2O splashes into from fluid flow tube, by the pH value of aqueous solution of urea conditioned reaction liquid, it is remained between 7.5～8.0, and under 75 ℃ temperature condition, reaction 2h makes Al (OH)
3Be coated on nanometer SiO
2Particle surface after reaction finishes, is used earlier deionized water wash, with the dehydrated alcohol dehydration, under 110 ℃ temperature condition, be dried to constant weight then again, use earlier deionized water wash, with the dehydrated alcohol dehydration, under 110 ℃ temperature condition, be dried to constant weight then again, promptly make the surface and coat Al (OH)
3Nanometer SiO
2Powder.
Second step. organically-modified: as earlier to be that 0.5% Sodium dodecylbenzene sulfonate (SDBS) adds and has in the reactor of whipping appts with mass percent, add a certain amount of deionized water then, after treating its stirring and dissolving, be the above-mentioned surface coating Al (OH) that makes of proportioning adding of 50g/L by solid-to-liquid ratio
3Nanometer SiO
2Powder, the pH=6 of conditioned reaction liquid, stirring reaction 2h, after reaction finishes, use deionized water wash earlier, dewater with dehydrated alcohol again, under 110 ℃ temperature condition, be dried to constant weight then, promptly make through surface of aluminum hydroxide and coat the nanometer SiO of Sodium dodecylbenzene sulfonate surface modification
2Powder.
Embodiment 2
According to the processing method of embodiment 1, Al (NO
3)
39H
2The concentration of O is 0.03mol/L, and the add-on of Sodium dodecylbenzene sulfonate (SDBS) is 1.0% (wt%).
Embodiment 3
According to the processing method of embodiment 1, Al (NO
3)
39H
2The concentration of O is 0.03mol/L, and the add-on of Sodium dodecylbenzene sulfonate (SDBS) is 1.5% (wt%).
Embodiment 4
According to the processing method of embodiment 1, Al (NO
3)
39H
2The concentration of O is 0.03mol/L, and the add-on of Sodium dodecylbenzene sulfonate (SDBS) is 2.0% (wt%).
Embodiment 5
According to the processing method of embodiment 1, Al (NO
3)
39H
2The concentration of O is 0.05mol/L, and the add-on of Sodium dodecylbenzene sulfonate (SDBS) is 0.5% (wt%).
Embodiment 6
According to the processing method of embodiment 1, Al (NO
3)
39H
2The concentration of O is 0.05mol/L, and the add-on of Sodium dodecylbenzene sulfonate (SDBS) is 1.0% (wt%).
Embodiment 7
According to the processing method of embodiment 1, Al (NO
3)
39H
2The concentration of O is 0.05mol/L, and the add-on of Sodium dodecylbenzene sulfonate (SDBS) is 1.5% (wt%).
Embodiment 8
According to the processing method of embodiment 1, Al (NO
3)
39H
2The concentration of O is 0.05mol/L, and the add-on of Sodium dodecylbenzene sulfonate (SDBS) is 2.0% (wt%).
Embodiment 9
According to the processing method of embodiment 1, Al (NO
3)
39H
2The concentration of O is 0.07mol/L, and the add-on of Sodium dodecylbenzene sulfonate (SDBS) is 0.5% (wt%).
Embodiment 10
According to the processing method of embodiment 1, Al (NO
3)
39H
2The concentration of O is 0.07mol/L, and the add-on of Sodium dodecylbenzene sulfonate (SDBS) is 1.0% (wt%).
Embodiment 11
According to the processing method of embodiment 1, Al (NO
3)
39H
2The concentration of O is 0.07mol/L, and the add-on of Sodium dodecylbenzene sulfonate (SDBS) is 1.5% (wt%).
Embodiment 12
According to the processing method of embodiment 1, Al (NO
3)
39H
2The concentration of O is 0.07mol/L, and the add-on of Sodium dodecylbenzene sulfonate (SDBS) is 2.0% (wt%).
Embodiment 13
According to the processing method of embodiment 1, Al (NO
3)
39H
2The concentration of O is for O.1mol/L, and the add-on of Sodium dodecylbenzene sulfonate (SDBS) is 0.5% (wt%).
Embodiment 14
According to the processing method of embodiment 1, Al (NO
3)
39H
2The concentration of O is 0.1mol/L, and the add-on of Sodium dodecylbenzene sulfonate (SDBS) is 1.0% (wt%).
Embodiment 15
According to the processing method of embodiment 1, Al (NO
3)
39H
2The concentration of O is 0.1mol/L, and the add-on of Sodium dodecylbenzene sulfonate (SDBS) is 1.5% (wt%).
Embodiment 16
According to the processing method of embodiment 1, Al (NO
3)
39H
2The concentration of O is 0.1mol/L, and the add-on of Sodium dodecylbenzene sulfonate (SDBS) is 2.0% (wt%).
Embodiment 17
Al (NO
3)
39H
2The concentration of O is 0.05mol/L, and the add-on of Sodium dodecylbenzene sulfonate (SDBS) is 1.0% (wt%).
Claims (1)
1. nanometer SiO
2The dispersing method of powder body material is characterized in that this method follows these steps to carry out successively:
The first step, inorganic coating: in the reactor that has whipping appts and fluid flow tube, adding the 1L solid-to-liquid ratio is the nanometer SiO of 50g/L
2Colloidal sol stirs, and is the Al (NO of 0.02～0.1mol/L again with 20ml concentration
3)
39H
2O splashes into from fluid flow tube, pH value with aqueous solution of urea conditioned reaction liquid, it is remained between 7.5～8.0, under 75 ℃ temperature condition, reaction 2h is after reaction finishes, use deionized water wash, dewater with dehydrated alcohol again, and then under 110 ℃ temperature, be dried to constant weight, promptly make the surface and coat Al (OH)
3Nanometer SiO
2Powder;
Second step, organically-modified: with mass percent is that 0.5%～2.0% Sodium dodecylbenzene sulfonate adds and has in the reactor of whipping appts, after adding the dissolving evenly of 1L deionized water and stirring, be the above-mentioned surface coating Al (OH) that makes of proportioning adding of 50g/L by solid-to-liquid ratio
3Nanometer SiO
2Powder, the pH=6 of conditioned reaction liquid, stirring reaction 2h, after reaction finishes, use deionized water wash earlier, dewater with dehydrated alcohol again, under 110 ℃ temperature condition, be dried to constant weight then, promptly make the nanometer SiO that surface of aluminum hydroxide coats the Sodium dodecylbenzene sulfonate surface modification
2Powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100129460A CN100457833C (en) | 2005-10-26 | 2005-10-26 | Nanometer SiO2 powder dispersion method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100129460A CN100457833C (en) | 2005-10-26 | 2005-10-26 | Nanometer SiO2 powder dispersion method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1757681A true CN1757681A (en) | 2006-04-12 |
| CN100457833C CN100457833C (en) | 2009-02-04 |
Family
ID=36703257
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100129460A Expired - Fee Related CN100457833C (en) | 2005-10-26 | 2005-10-26 | Nanometer SiO2 powder dispersion method |
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|---|---|
| CN (1) | CN100457833C (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107032358A (en) * | 2017-04-07 | 2017-08-11 | 华侨大学 | A kind of method that silica particles coat alundum (Al2O3) |
| CN110527284A (en) * | 2019-09-03 | 2019-12-03 | 王良仁 | A kind of automobile plating nylon plastic material and preparation method |
| CN114539811A (en) * | 2022-03-01 | 2022-05-27 | 昆明冶金研究院有限公司 | High-covering-performance easily-dispersible silica fume and preparation method thereof |
| CN114539810A (en) * | 2022-03-01 | 2022-05-27 | 昆明冶金研究院有限公司 | High-dispersion modified silica fume and preparation method thereof |
| CN114539815A (en) * | 2022-03-01 | 2022-05-27 | 昆明冶金研究院有限公司 | High-covering high-dispersity modified micro silicon powder and preparation method thereof |
| CN116769392A (en) * | 2023-07-17 | 2023-09-19 | 深圳市深赛尔股份有限公司 | Water-based paint for metal color steel plate surface and preparation method thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BR9405723A (en) * | 1993-02-12 | 1995-11-28 | Cabot Corp | Manufacturing process of surfactant-modified silica material |
| JPH06299087A (en) * | 1993-04-15 | 1994-10-25 | Matsushita Electric Works Ltd | Sealing material and its production |
| CN1141341C (en) * | 2001-01-21 | 2004-03-10 | 天津大学 | Surface treating process for modifying nm-class oxide powder |
| JP2005162771A (en) * | 2003-11-28 | 2005-06-23 | Showa Aluminum Powder Kk | Compositely coated aluminum pigment |
-
2005
- 2005-10-26 CN CNB2005100129460A patent/CN100457833C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107032358A (en) * | 2017-04-07 | 2017-08-11 | 华侨大学 | A kind of method that silica particles coat alundum (Al2O3) |
| CN110527284A (en) * | 2019-09-03 | 2019-12-03 | 王良仁 | A kind of automobile plating nylon plastic material and preparation method |
| CN114539811A (en) * | 2022-03-01 | 2022-05-27 | 昆明冶金研究院有限公司 | High-covering-performance easily-dispersible silica fume and preparation method thereof |
| CN114539810A (en) * | 2022-03-01 | 2022-05-27 | 昆明冶金研究院有限公司 | High-dispersion modified silica fume and preparation method thereof |
| CN114539815A (en) * | 2022-03-01 | 2022-05-27 | 昆明冶金研究院有限公司 | High-covering high-dispersity modified micro silicon powder and preparation method thereof |
| CN116769392A (en) * | 2023-07-17 | 2023-09-19 | 深圳市深赛尔股份有限公司 | Water-based paint for metal color steel plate surface and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN100457833C (en) | 2009-02-04 |
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| C06 | Publication | ||
| PB01 | Publication | ||
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| 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: Guangdong Smith Technology Co.,Ltd. Assignor: Taiyuan University of Technology Contract fulfillment period: 2009.3.24 to 2014.4.24 contract change Contract record no.: 2010440000123 Denomination of invention: Nanometer SiO2 powder dispersion method Granted publication date: 20090204 License type: Exclusive license Record date: 2010.1.6 |
|
| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.3.24 TO 2014.4.24; CHANGE OF CONTRACT Name of requester: GUANGDONG JINGHUA TECHNOLOGY CO.,LTD Effective date: 20100106 |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
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Granted publication date: 20090204 Termination date: 20161026 |