CN101914313A - Cation water-based nano silicon dioxide and preparation method and application thereof - Google Patents
Cation water-based nano silicon dioxide and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses cation water-based nano silicon dioxide and preparation method and application thereof. When in preparation, water, octadecyl dimethyl benzyl ammonium chloride and concentrated hydrochloric acid are added into a reactor to be stirred and dissolved; nano silicon dioxide micro powder is added into the reactor, stirring is carried out, so as to obtain low viscosity semi-transparent solution, and aminosilane coupling agent is dropwise added into the reactor while stirring; the pH value of the solution is regulated to 3-4, and the solution is continuously stirred, so as to obtain semi-transparent cation water-based nano silicon dioxide. The invention provides a cation surfactant and an aminosilane coupling agent into water phase, the surface characteristic of nano silicon dioxide and rheological property of dispersion are effectively improved, a nano silicon dioxide water-based dispersion with low viscosity, high stability and high uniformity is obtained, and further a high light waterproof coating slurry can be prepared.
Description
Technical field:
The present invention relates to the cation-modified product of a kind of nano-silica surface and preparation method and purposes.
Background technology:
Nano material is meant that the three-dimensional space yardstick has at least one dimension to be in the material of nanometer scale (1-100nm), the material of new generation that it is made up of the nanoparticle of size between atom, molecule and meta system.The corresponding nanotechnology that grows up of nano material is acknowledged as the scientific research field that 21 century has future most.Nano silicon claims " ultra-fine white carbon black " again, have characteristics such as particle diameter is little, specific surface area is big, chemical purity is high, dispersing property is good, it has superior stability, reinforcement, thickening property and thixotropy simultaneously, can improve other material or product inherent physical attribute and chemical property, be industries such as rubber, chemical industry, light industry, weaving, electronics, machinery, food, medicine, the agricultural indexs needed " industrial monosodium glutamate " of improving the quality of products.It is widely used in catalyzer, support of the catalyst, petrochemical complex, discoloring agent, matting agent, rubber reinforcing filler, plastics filling agent, printing ink thickening material, the soft polishing agent of metal, insulation and thermal insulation weighting agent, various fields such as high-grade daily-use makeup filler and spray material.Along with modern society's constant development of economy, to the demand of nano silicon with increasing.
But nano-silica surface has a large amount of hydroxyls, and planar water and higher specific surface energy are easy to generate and reunite or flocculation, influence the stability and the homogeneity of dispersion liquid.
Summary of the invention:
The object of the present invention is to provide a kind of good stability, cation water-based nano silicon dioxide of good uniformity and its production and use.
Technical solution of the present invention is:
A kind of cation water-based nano silicon dioxide is characterized in that: made by following method:
1) water and stearyl dimethyl benzyl ammonium chloride, concentrated hydrochloric acid are added in the reactor stirring and dissolving;
2) the nanometer titanium dioxide silicon powder is added in the reactor, stir and obtain the translucent solution of low viscosity;
3) in step 2) stir in, amino silicane coupling agent is added drop-wise in the reactor;
4) regulator solution pH value to 3～4 are continued stirred solution and are obtained translucent cation water-based nano silicon dioxide.
A kind of preparation method of cation water-based nano silicon dioxide is characterized in that: comprise the following steps: successively
1) water and stearyl dimethyl benzyl ammonium chloride, concentrated hydrochloric acid are added in the reactor stirring and dissolving;
2) the nanometer titanium dioxide silicon powder is added in the reactor, stir and obtain the translucent solution of low viscosity;
3) in step 2) stir in, amino silicane coupling agent is added drop-wise in the reactor;
4) regulator solution pH value to 3～4 are continued stirred solution and are obtained translucent cation water-based nano silicon dioxide.
The preparation method of described cation water-based nano silicon dioxide comprises the following steps: successively
1) in open reactor, adds 230 weight parts waters under 5-40 ℃, again 6 weight part stearyl dimethyl benzyl ammonium chlorides and 3 weight parts, 37% mass concentration concentrated hydrochloric acid are added wherein, stir dissolving in 5 minutes;
2) the nanometer titanium dioxide silicon powder with 60 weight part particle diameter 10-100nm adds in the reactor, and the 4000r/min high-speed stirring obtained the translucent solution of low viscosity in 5 minutes;
3) in step 2) in the high-speed stirring, 6 weight part amino silicane coupling agents are added drop-wise in the reactor, drip time 10min;
4) stirred solution was continued 10 minutes in regulator solution pH value to 3～4, obtained translucent cation water-based nano silicon dioxide.
Amino silicane coupling agent is one or more in 3-aminopropyl trimethoxysilane, 3-aminopropyl triethoxysilane, 3-methacryloxypropyl trimethoxy silane, the 3-mercaptopropyl trimethoxysilane.
The application of a kind of cation water-based nano silicon dioxide in preparation high-gloss water-proof coating paste, it is characterized in that: at room temperature, the cation water-based nano silicon dioxide that adds 300g solid content 20% in the open reactor, add 60g ethanol in the time of the 2000r/min high-speed stirring, the PVA of 100g solid content 15% (polyvinyl alcohol) solution, 0.6g white dyes, 0.02g water-based flow agent reach, 0.2g linking agent, mix, filter, obtain translucent coating fluid, i.e. the high-gloss water-proof coating paste.
The described PVA polymerization degree is more than 2000.
The water-based flow agent is a polyether modified siloxane class tensio-active agent.
Linking agent is one or more in maleic anhydride, phthalyl chloride, phthalate anhydride, Pyroglutaric acid, Succinic anhydried, phthalic acid, epoxy chloropropane, formaldehyde, potassium permanganate, hydroxide mantoquita, chromic salts, vanadic salts, the zirconates.
The present invention is by the introducing at a kind of cats product of aqueous phase and a kind of amino silicane coupling agent, the surface property of nano silicon and the rheological of dispersion liquid have effectively been improved, obtained a kind of low viscosity, high stability, the nano silicon aqueous liquid dispersion of high uniformity (being cation water-based nano silicon dioxide), and can make a kind of high-gloss water-proof coating paste thus.
The invention will be further described below in conjunction with drawings and Examples.
Fig. 1 is the projection Electronic Speculum figure of nano silicon before the modification.
Fig. 2 is the projection Electronic Speculum figure of nano silicon after the modification.
Embodiment:
Embodiment 1:
1) in open reactor, adds 230 weight parts waters under 5-40 ℃, again 6 weight part stearyl dimethyl benzyl ammonium chlorides and 3 weight parts, 37% mass concentration concentrated hydrochloric acid are added wherein, stir dissolving in 5 minutes;
2) the nanometer titanium dioxide silicon powder with 60 weight part particle diameter 10-100nm adds in the reactor, and the 4000r/min high-speed stirring obtained the translucent solution of low viscosity in 5 minutes;
3) in step 2) in the high-speed stirring, 6 weight part amino silicane coupling agents are added drop-wise in the reactor, drip time 10min;
4) regulator solution pH value to 3～4 continued stirred solutions 10 minutes, obtained translucent cation water-based nano silicon dioxide (being the nano silicon dispersion liquid), and this dispersion liquid at room temperature can be placed more than 6 months not gel.
Amino silicane coupling agent is 3-aminopropyl trimethoxysilane (or in the 3-aminopropyl triethoxysilane, 3-methacryloxypropyl trimethoxy silane, 3-mercaptopropyl trimethoxysilane one or more).
The application of a kind of cation water-based nano silicon dioxide in preparation high-gloss water-proof coating paste, at room temperature, the cation water-based nano silicon dioxide that adds 300g solid content 20% in the open reactor, add 60g ethanol in the time of the 2000r/min high-speed stirring, the PVA of 100g solid content 15% (polyvinyl alcohol) solution, 0.6g white dyes, 0.02g water-based flow agent reach the 0.2g linking agent, mix, filter, obtain translucent coating fluid, i.e. the high-gloss water-proof coating paste.
The described PVA polymerization degree is more than 2000.
The water-based flow agent is a polyether modified siloxane class tensio-active agent.
Linking agent is maleic anhydride (or in the phthalyl chloride, phthalate anhydride, Pyroglutaric acid, Succinic anhydried, phthalic acid, epoxy chloropropane, formaldehyde, potassium permanganate, hydroxide mantoquita, chromic salts, vanadic salts, zirconates one or more).
Claims (8)
1. cation water-based nano silicon dioxide is characterized in that: made by following method:
1) water and stearyl dimethyl benzyl ammonium chloride, concentrated hydrochloric acid are added in the reactor stirring and dissolving;
2) the nanometer titanium dioxide silicon powder is added in the reactor, stir and obtain the translucent solution of low viscosity;
3) in step 2) stir in, amino silicane coupling agent is added drop-wise in the reactor;
4) regulator solution pH value to 3～4 are continued stirred solution and are obtained translucent cation water-based nano silicon dioxide.
2. the preparation method of a cation water-based nano silicon dioxide is characterized in that: comprise the following steps: successively
1) water and stearyl dimethyl benzyl ammonium chloride, concentrated hydrochloric acid are added in the reactor stirring and dissolving;
2) the nanometer titanium dioxide silicon powder is added in the reactor, stir and obtain the translucent solution of low viscosity;
3) in step 2) stir in, amino silicane coupling agent is added drop-wise in the reactor;
4) regulator solution pH value to 3～4 are continued stirred solution and are obtained translucent cation water-based nano silicon dioxide.
3. the preparation method of cation water-based nano silicon dioxide according to claim 4 is characterized in that: comprise the following steps: successively
1) in open reactor, adds 230 weight parts waters under 5-40 ℃, again 6 weight part stearyl dimethyl benzyl ammonium chlorides and 3 weight parts, 37% mass concentration concentrated hydrochloric acid are added wherein, stir dissolving in 5 minutes;
2) the nanometer titanium dioxide silicon powder with 60 weight part particle diameter 10-100nm adds in the reactor, and the 4000r/min high-speed stirring obtained the translucent solution of low viscosity in 5 minutes;
3) in step 2) in the high-speed stirring, 6 weight part amino silicane coupling agents are added drop-wise in the reactor, drip time 10min;
4) stirred solution was continued 10 minutes in regulator solution pH value to 3～4, obtained translucent cation water-based nano silicon dioxide.
4. according to the preparation method of claim 2 or 3 described cation water-based nano silicon dioxides, it is characterized in that: amino silicane coupling agent is one or more in 3-aminopropyl trimethoxysilane, 3-aminopropyl triethoxysilane, 3-methacryloxypropyl trimethoxy silane, the 3-mercaptopropyl trimethoxysilane.
5. the application of the described cation water-based nano silicon dioxide of claim 1 in preparation high-gloss water-proof coating paste, it is characterized in that: at room temperature, the cation water-based nano silicon dioxide that adds 300g solid content 20% in the open reactor, add 60g ethanol in the time of the 2000r/min high-speed stirring, the PVA solution of 100g solid content 15%, 0.6g white dyes, 0.02g water-based flow agent reach, 0.2g linking agent, mix, filter, obtain translucent coating fluid, i.e. the high-gloss water-proof coating paste.
6. the application of cation water-based nano silicon dioxide according to claim 5 in preparation high-gloss water-proof coating paste, it is characterized in that: the described PVA polymerization degree is more than 2000.
7. the application in preparation high-gloss water-proof coating paste according to claim 5 or 6 described cation water-based nano silicon dioxides, it is characterized in that: the water-based flow agent is a polyether modified siloxane class tensio-active agent.
8. the application in preparation high-gloss water-proof coating paste according to claim 5 or 6 described cation water-based nano silicon dioxides, it is characterized in that: linking agent is one or more in maleic anhydride, phthalyl chloride, phthalate anhydride, Pyroglutaric acid, Succinic anhydried, phthalic acid, epoxy chloropropane, formaldehyde, potassium permanganate, hydroxide mantoquita, chromic salts, vanadic salts, the zirconates.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102500414A (en) * | 2011-11-17 | 2012-06-20 | 上海华谊（集团）公司 | Organic amine solid basic catalyst as well as preparation method and application thereof |
| CN102501674A (en) * | 2011-10-14 | 2012-06-20 | 江苏格美高科技发展有限公司 | Glossy waterproof polypropylene photo paper applicable for aqueous ink and its preparation method |
| CN102558916A (en) * | 2011-12-16 | 2012-07-11 | 天津大学 | Nano silicon dioxide particle surface modifying method based on charge environment control and application thereof |
| CN102675929A (en) * | 2012-04-17 | 2012-09-19 | 淮阴工学院 | Preparation method of fluorescent composite whitened attapulgite |
| CN103013182A (en) * | 2012-12-06 | 2013-04-03 | 常州大学 | Surface modification method of nanosilicon dioxide |
| CN104099013A (en) * | 2014-06-19 | 2014-10-15 | 锐展(铜陵)科技有限公司 | Nano aluminium alloy surface treating agent |
| CN104761929A (en) * | 2014-12-09 | 2015-07-08 | 西南石油大学 | Modified nanometer SiO2 monomer used for polymer flooding |
| CN108333168A (en) * | 2018-04-28 | 2018-07-27 | 厦门斯贝克科技有限责任公司 | A kind of enhancing Raman detection method using satellite structure |
| CN108862288A (en) * | 2018-07-26 | 2018-11-23 | 安徽锦华氧化锌有限公司 | A kind of processing method of yellowing-resistant white carbon black |
| CN109456746A (en) * | 2017-09-06 | 2019-03-12 | 中国石油化工股份有限公司 | A kind of nanometer wetting agent and its preparation method and application based on cationic surfactant modification |
| CN113416431A (en) * | 2021-06-23 | 2021-09-21 | 上海兴赛尔表面材料有限公司 | Preparation method of environment-friendly anticorrosive pigment with self-repairing function |
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| WO2003055799A1 (en) * | 2001-12-25 | 2003-07-10 | Asahi Kasei Chemicals Corporation | Inorganic porous fine particles |
| CN1536032A (en) * | 2003-04-07 | 2004-10-13 | 章浩龙 | Nano silicon dioxide emulsion, its preparation method and application |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2003055799A1 (en) * | 2001-12-25 | 2003-07-10 | Asahi Kasei Chemicals Corporation | Inorganic porous fine particles |
| CN1608031A (en) * | 2001-12-25 | 2005-04-20 | 旭化成化学株式会社 | Inorganic porous fine particles |
| CN1536032A (en) * | 2003-04-07 | 2004-10-13 | 章浩龙 | Nano silicon dioxide emulsion, its preparation method and application |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102501674A (en) * | 2011-10-14 | 2012-06-20 | 江苏格美高科技发展有限公司 | Glossy waterproof polypropylene photo paper applicable for aqueous ink and its preparation method |
| CN102500414B (en) * | 2011-11-17 | 2014-12-10 | 上海华谊（集团）公司 | Organic amine solid basic catalyst as well as preparation method and application thereof |
| CN102500414A (en) * | 2011-11-17 | 2012-06-20 | 上海华谊（集团）公司 | Organic amine solid basic catalyst as well as preparation method and application thereof |
| CN102558916A (en) * | 2011-12-16 | 2012-07-11 | 天津大学 | Nano silicon dioxide particle surface modifying method based on charge environment control and application thereof |
| CN102558916B (en) * | 2011-12-16 | 2013-08-07 | 天津大学 | Nano silicon dioxide particle surface modifying method based on charge environment control and application thereof |
| CN102675929A (en) * | 2012-04-17 | 2012-09-19 | 淮阴工学院 | Preparation method of fluorescent composite whitened attapulgite |
| CN102675929B (en) * | 2012-04-17 | 2013-12-04 | 淮阴工学院 | Preparation method of fluorescent composite whitened attapulgite |
| CN103013182A (en) * | 2012-12-06 | 2013-04-03 | 常州大学 | Surface modification method of nanosilicon dioxide |
| CN104099013A (en) * | 2014-06-19 | 2014-10-15 | 锐展(铜陵)科技有限公司 | Nano aluminium alloy surface treating agent |
| CN104099013B (en) * | 2014-06-19 | 2016-07-06 | 锐展(铜陵)科技有限公司 | A kind of nano-aluminium alloy surface conditioning agent |
| CN104761929A (en) * | 2014-12-09 | 2015-07-08 | 西南石油大学 | Modified nanometer SiO2 monomer used for polymer flooding |
| CN104761929B (en) * | 2014-12-09 | 2017-04-12 | 西南石油大学 | Modified nanometer SiO2 monomer used for polymer flooding |
| CN109456746A (en) * | 2017-09-06 | 2019-03-12 | 中国石油化工股份有限公司 | A kind of nanometer wetting agent and its preparation method and application based on cationic surfactant modification |
| CN108333168A (en) * | 2018-04-28 | 2018-07-27 | 厦门斯贝克科技有限责任公司 | A kind of enhancing Raman detection method using satellite structure |
| CN108862288A (en) * | 2018-07-26 | 2018-11-23 | 安徽锦华氧化锌有限公司 | A kind of processing method of yellowing-resistant white carbon black |
| CN113416431A (en) * | 2021-06-23 | 2021-09-21 | 上海兴赛尔表面材料有限公司 | Preparation method of environment-friendly anticorrosive pigment with self-repairing function |
| CN113416431B (en) * | 2021-06-23 | 2022-06-10 | 上海兴赛尔表面材料有限公司 | Preparation method of environment-friendly anticorrosive pigment with self-repairing function |
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