CN102660154A - Surface modification method for nanometer titanium dioxide - Google Patents
Surface modification method for nanometer titanium dioxide Download PDFInfo
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- CN102660154A CN102660154A CN2012101287300A CN201210128730A CN102660154A CN 102660154 A CN102660154 A CN 102660154A CN 2012101287300 A CN2012101287300 A CN 2012101287300A CN 201210128730 A CN201210128730 A CN 201210128730A CN 102660154 A CN102660154 A CN 102660154A
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Abstract
The invention belongs to the technical field of powder processing and relates to a surface modification method for nanometer titanium dioxide, in particular to a method for modifying the nanometer titanium dioxide surface by using a silane coupling agent and accordingly improving the dispersibility and the lipophilicity of titanium dioxide. The surface modification method for the nanometer titanium dioxide has the advantages and the effects that by adopting the scheme, the number of hydroxyls on the surfaces of nanometer titanium dioxide particles is decreased, the nanometer titanium dioxide particles and polar groups of the silane coupling agent react, and organic chains are formed on the surfaces of the nanometer titanium dioxide particles through hydrophobization, so that the hydrophilia of the nanometer titanium dioxide is changed into the lipophilicity. In addition, conglomeration of the particles is reduced, the dispersibility of the nanometer titanium dioxide in an organic phase is improved, and the application range of the nanometer titanium dioxide is widened accordingly. The surface modification method for the nanometer titanium dioxide is simple in operation, low in cost and free of pollution.
Description
Technical field
The present invention relates to a kind of surface modification method of nano titanium oxide, is through a kind of silane coupling agent titanium dioxide surface to be carried out modification specifically, thereby improves dispersiveness, the oleophilicity of titanium oxide, belongs to the powder processing technical field.
Background technology
Nano titanium oxide (TiO
2) be the very high function fine inorganic material of a kind of faster added value of development in recent years, to have a particle diameter little because of it, and specific surface area is big; Magnetic is strong, and photochemical catalysis, absorptive character are good, and it is strong to absorb ultraviolet ability; Surfactivity is big; Heat conductance is good, good dispersivity, and good weather resisteant, chemical resistance; Characteristics such as anti-uv-ray is strong are widely used in fields such as sensitive materials, photocatalyst, makeup, packaging material for food, ceramic additive, rubber, plastics, leather tanning, sedan limousine coating.
But because the surface energy of nanometer particle is high; Reunite easily, form primary particle, in organic phase, be difficult to shortcomings such as infiltration and dispersion stabilization difference; Can't show nano-meter characteristics such as gratifying big specific area effect, volume effect and quantum size effect; Therefore for the consistency of improving nano titanium oxide and organic system and at the dispersion stabilization of organic system, improve the over-all properties of the compound system of interpolation nano titanium oxide, must carry out surface-treated it; Through changing the physico-chemical property on nano titanium oxide surface, improve itself and the consistency and the bonding force of organic molecule, widen its Application Areas, therefore, the modification processing is carried out on the nano-titania particle surface had very important and practical meanings.
Summary of the invention
The object of the invention is to make the polar group of silane coupling agent KH-560 and the functional group reactions on titanium dioxide nanoparticle surface to form stable chemical bond, thereby improves its dispersiveness and oleophilicity; The mechanism of KH560 decorated nanometer titanium oxide mainly be titanic oxide material surface hydroxyl under certain condition with the functional group of the epoxy silane coupling agent generation covalent linkage that reacts; Its principal reaction mechanism mainly is: having under the water condition, the methoxyl group in the KH-560 molecule generates Si-OH (hydrolysis reaction is shown in the figure l) with water molecules effect hydrolysis earlier; Si-OH that generates and titanium dioxide surface-OH generation shrink reaction, form Ti-O-Si key bonding reaction, (shown in Figure 2) and organic chain in the nanoparticle surface grafting.
The silane coupling agent KH-560 of bibliographical information generally is used for the surface-treated of nano silicon at present, and the modification that is used for nano titanium oxide relatively could be accomplished under the exacting terms; And this experiment shows, in aqueous conditions, effect in the time of through ultrasonic and stirring increases coupling agent molecule and nano-titania particle collision opportunity, thereby shortened the bonding time, improves modified effect; Silane coupling agent KH-560 is firm is bonded in the nano-titanium dioxide powder surface; And introduction specific functional groups; Wettability and the dispersiveness of nano titanium oxide in polymkeric substance is improved; Also widened its range of application, this patent provides the KH-560 modified nano-titanium dioxide comparatively gentle modified condition.
The present invention accomplishes through following technical proposal: a kind of nano titanium oxide surface modification method, and its characteristic makes through following step:
A, 5 weight part nano titanium dioxide powders are joined in the mixing solutions of 90 weight part absolute ethyl alcohols and 10 parts by weight of deionized water, obtain mixing solutions 1;
B, 1 li of mixing solutions, press 1% of nano titanium dioxide powder quality and add dispersion agent, sonic oscillation fully disperses dispersion agent then, obtains mixing solutions 2;
C, in mixing solutions 2, add PH that Glacial acetic acid min. 99.5 makes mixing solutions 2 between 3.5-5.5, obtain mixing solutions 3;
D, the KH-560 of the 5%-50% of nano titanium dioxide powder quality is added in the mixing solutions 3, and stir with ultrasonic concussion fast simultaneously and make KH-560 fully disperse, obtain mixing solutions 4;
E, mixing solutions 4 is heated to 80 ℃, stirs, constant temperature refluxed 2 hours, obtained mixed slurry;
F, mixed slurry is carried out alcohol by routine wash, washing, oven dry after the grinding, obtains the nano titanium oxide of modification.
The dispersion agent of said step B is the TAZ-ND1 dispersion agent.
The silane coupling agent trade mark among the said step C is KH-560, i.e. γ-glycidyl ether oxygen propyl trimethoxy silicane.
The present invention has the following advantages and effect: adopt such scheme; Nano-titania particle surface hydroxyl quantity reduces, with the polar group reaction of silane coupling agent, and on its surface grafting hydrophobic organic chain; Make nano titanium oxide from the hydrophilic oleophylic that is transformed into like this; And reduced interparticle reunion, improved the dispersiveness of nano titanium oxide in organic phase, and then widened its range of application; The present invention is simple to operate, and is with low cost, pollution-free.
Description of drawings
Fig. 1Hydrolysis reaction schematic diagram for the KH-560 molecule;
Fig. 2Be TiO
2And the bonding reaction schematic diagram between silane coupling agent;
Fig. 3For unmodified nano titanium oxide (Fig. 3 a) with the infrared spectrum of the nano titanium oxide (Fig. 3 b) of silane coupling agent KH-560 modification;
Fig. 4The TEM photo of nano titanium oxide, Fig. 4 (a) are the TEM photo of modified nano-titanium dioxide; Fig. 4 (b) is the TEM photo of unmodified nano titanium oxide.
Embodiment
Below in conjunction with concrete mode the present invention is further specified:
Embodiment 1
A, the 5g nano titanium dioxide powder is joined in the mixing solutions of 90g absolute ethyl alcohol and 10g deionized water, obtain mixing solutions 1;
B, 1 li of mixing solutions, add the 0.05g dispersion agent, sonic oscillation 30min fully disperses dispersion agent then, obtains mixing solutions 2;
C, in mixing solutions 2, adding Glacial acetic acid min. 99.5, to make the pH value of mixing solutions 2 be 3.5, obtains mixing solutions 3;
D, 0.5gKH-560 is joined mixing solutions 3, and stir and ultrasonic concussion 30min fast simultaneously, obtain mixing solutions 4;
E, mixing solutions 4 is heated to 80 ℃, stirs, constant temperature refluxed 2 hours, obtained mixed slurry;
F, mixed slurry is carried out alcohol by routine wash, washing, oven dry after the grinding, obtains the nano titanium oxide of modification.
Embodiment 2
A, the 5g nano titanium dioxide powder is joined in the mixing solutions of 90g absolute ethyl alcohol and 10g deionized water, obtain mixing solutions 1;
B, 1 li of mixing solutions, add the 0.05g dispersion agent,, sonic oscillation 30min fully disperses dispersion agent then, obtains mixing solutions 2;
C, in mixing solutions 2, adding Glacial acetic acid min. 99.5, to make the PH of system be 4.5, obtains mixing solutions 3;
D, 1.0gKH-560 is joined mixing solutions 3, and stir and ultrasonic concussion 30min fast simultaneously, obtain mixing solutions 4;
E, mixing solutions 4 is heated to 80 ℃, stirs, constant temperature refluxed 2 hours, obtained mixed slurry;
F, mixed slurry is carried out alcohol by routine wash, washing, oven dry after the grinding, obtains the nano titanium oxide of modification.
Embodiment 3
The nano titanium oxide of surface-treated provided by the invention, the following step gained of process:
A, the 5g nano titanium dioxide powder is joined in the mixing solutions of 90g absolute ethyl alcohol and 10g deionized water, obtain mixing solutions 1;
B, 1 li of mixing solutions, add the 0.05g dispersion agent, sonic oscillation 30min fully disperses dispersion agent then, obtains mixing solutions 2;
C, in mixing solutions 2, adding Glacial acetic acid min. 99.5, to make the PH of system be 5.5, obtains mixing solutions 3;
D, 2.0gKH-560 is joined mixing solutions 3, and stir and ultrasonic concussion 30min fast simultaneously, obtain mixing solutions 4;
E, mixing solutions 4 is heated to 80 ℃, stirs, constant temperature refluxed 2 hours, obtained mixed slurry;
F, mixed slurry is carried out alcohol by routine wash, washing, oven dry after the grinding, obtains the nano titanium oxide of modification.
Embodiment 4
The nano titanium oxide of surface-treated provided by the invention, the following step gained of process:
A, the 5g nano titanium dioxide powder is joined in the mixing solutions of 90g absolute ethyl alcohol and 10g deionized water, obtain mixing solutions 1;
B, 1 li of mixing solutions, add the 0.05g dispersion agent, sonic oscillation 30min fully disperses dispersion agent then, obtains mixing solutions 2;
C, in mixing solutions 2, adding Glacial acetic acid min. 99.5, to make the PH of system be 4.5, obtains mixing solutions 3;
D, 1.5gKH-560 is joined mixing solutions 3, and stir and ultrasonic concussion 30min fast simultaneously, obtain mixing solutions 4;
E, mixing solutions 4 is heated to 80 ℃, stirs, constant temperature refluxed 2 hours, obtained mixed slurry;
F, mixed slurry is carried out alcohol by routine wash, washing, oven dry after the grinding, obtains the nano titanium oxide of modification.
The nanoparticle of institute's modification is observed nanoparticle surface functional group, size, deployment conditions with FFIR (FT-IR), transmission electron microscope (TEM).
Fourier transformation infrared spectrometer (FT-IR) records the nano titanium dioxide powder infrared spectrum of silane coupling agent KH-560 modification, analyzes the absorption peak of its functional group; Fig. 3 be unmodified nano titanium oxide (Fig. 3 a) with the infrared spectrum of the nano titanium oxide (Fig. 3 b) of silane coupling agent KH-560 modification, by the 2926.84cm among Fig. 3 b
-1Tangible methylene radical vibration peak can be seen by the place, explains that silane coupling agent KH-560 has been bonded to the nano-titania particle surface.
(2) TEM characterizes
Nano titanium dioxide powder after the modification is scattered in the absolute ethyl alcohol, with the pattern of transmission electron microscope observation nanoparticle.Fig. 4 is the TEM photo of nano titanium oxide; Fig. 4 (a) is the TEM photo of modified nano-titanium dioxide, and the nano-titania particle after the modification is dispersed in the ethanol, does not have obvious agglomeration; Fig. 4 (b) is the TEM photo of unmodified nano titanium oxide, from figure, can obviously find out the nanoparticle serious agglomeration.Explain that the nano-titania particle after the modification can be scattered in the organic solvent preferably, effectively reduces the soft-agglomerated phenomenon of nanoparticle.
Claims (2)
1. nano titanium oxide surface modification method, its characteristic makes through following step:
A, 5 weight part nano titanium dioxide powders are joined in the mixing solutions of 90 weight part absolute ethyl alcohols and 10 parts by weight of deionized water, obtain mixing solutions 1;
B, 1 li of mixing solutions, press 1% of nano titanium dioxide powder quality and add dispersion agent, sonic oscillation fully disperses dispersion agent then, obtains mixing solutions 2;
C, in mixing solutions 2, add PH that Glacial acetic acid min. 99.5 makes mixing solutions 2 between 3.5-5.5, obtain mixing solutions 3;
D, the KH-560 of the 5%-50% of nano titanium dioxide powder quality is added in the mixing solutions 3, and stir with ultrasonic concussion fast simultaneously and make KH-560 fully disperse, obtain mixing solutions 4;
E, mixing solutions 4 is heated to 80 ℃, stirs, constant temperature refluxed 2 hours, obtained mixed slurry;
F, mixed slurry is carried out alcohol by routine wash, washing, oven dry after the grinding, obtains the nano titanium oxide of modification.
2. a kind of nano titanium oxide surface modification method as claimed in claim 1 is characterized in that: the dispersion agent of said step B is the TAZ-ND1 dispersion agent.
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| CN103087556A (en) * | 2012-12-31 | 2013-05-08 | 东莞市万钧化工新材料科技有限公司 | Surface treatment method and application of heat-conducting packing |
| CN103160148A (en) * | 2013-03-13 | 2013-06-19 | 复旦大学 | Surface-modified metal boride/Al2O3 multiphase ceramic powder and preparation method thereof |
| CN103525134A (en) * | 2013-09-22 | 2014-01-22 | 中国水产科学研究院东海水产研究所 | Surface modification method of nano-titanium dioxide |
| CN104140692A (en) * | 2014-07-10 | 2014-11-12 | 池州市英派科技有限公司 | Modified nano titanium dioxide with good hydrophobic effects and preparation method thereof |
| CN104745025A (en) * | 2014-08-22 | 2015-07-01 | 赵杰 | Environment-friendly type multifunctional nano modified coating and spraying method thereof |
| CN105694101A (en) * | 2016-01-30 | 2016-06-22 | 深圳市德宝五金塑胶有限公司 | Granular titanium dioxide and preparation method thereof |
| CN106046913A (en) * | 2016-07-29 | 2016-10-26 | 上海宇昂水性新材料科技股份有限公司 | Nanometer titania modified loading method and application |
| CN106587691A (en) * | 2016-10-28 | 2017-04-26 | 同济大学 | Method for preparing modified micro particles coated with graphene oxide |
| CN107142780A (en) * | 2017-05-15 | 2017-09-08 | 柳州博泽科技有限公司 | A kind of surface treatment method of nano titanium oxide applied to facing paper |
| CN109759040A (en) * | 2019-03-05 | 2019-05-17 | 辽宁石油化工大学 | A kind of preparation method of modifying titanium dioxide |
| CN110342900A (en) * | 2018-04-08 | 2019-10-18 | 江苏未名之光纳米科技有限公司 | A kind of height heat-barrier material and preparation method thereof |
| CN111607446A (en) * | 2020-06-30 | 2020-09-01 | 国网河南省电力公司新野县供电公司 | High-insulation high-stability modified transformer oil |
| CN112603838A (en) * | 2020-11-30 | 2021-04-06 | 上海蔻沣生物科技有限公司 | Nano titanium dioxide slurry oil and preparation method and application thereof |
| CN112981501A (en) * | 2021-03-05 | 2021-06-18 | 赵琳琳 | Composite bright nickel plating solution |
| CN113900169A (en) * | 2021-10-14 | 2022-01-07 | 宁波东旭成新材料科技有限公司 | Preparation method of anti-aging light diffusion film |
| CN114011476A (en) * | 2021-11-08 | 2022-02-08 | 四川大学 | Adsorption-catalytic decomposition integrated titanium dioxide and application thereof |
| CN114958034A (en) * | 2022-05-31 | 2022-08-30 | 龙佰禄丰钛业有限公司 | Preparation method of titanium dioxide organic composite coating for plastics |
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Cited By (21)
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| CN103087556A (en) * | 2012-12-31 | 2013-05-08 | 东莞市万钧化工新材料科技有限公司 | Surface treatment method and application of heat-conducting packing |
| CN103087556B (en) * | 2012-12-31 | 2014-11-12 | 东莞市万钧化工新材料科技有限公司 | Surface treatment method and application of heat-conducting packing |
| CN103160148A (en) * | 2013-03-13 | 2013-06-19 | 复旦大学 | Surface-modified metal boride/Al2O3 multiphase ceramic powder and preparation method thereof |
| CN103525134A (en) * | 2013-09-22 | 2014-01-22 | 中国水产科学研究院东海水产研究所 | Surface modification method of nano-titanium dioxide |
| CN104140692A (en) * | 2014-07-10 | 2014-11-12 | 池州市英派科技有限公司 | Modified nano titanium dioxide with good hydrophobic effects and preparation method thereof |
| CN104140692B (en) * | 2014-07-10 | 2016-01-20 | 池州市英派科技有限公司 | Modified nano-titanium dioxide that a kind of hydrophobic effect is good and preparation method thereof |
| CN104745025A (en) * | 2014-08-22 | 2015-07-01 | 赵杰 | Environment-friendly type multifunctional nano modified coating and spraying method thereof |
| CN105694101A (en) * | 2016-01-30 | 2016-06-22 | 深圳市德宝五金塑胶有限公司 | Granular titanium dioxide and preparation method thereof |
| CN106046913A (en) * | 2016-07-29 | 2016-10-26 | 上海宇昂水性新材料科技股份有限公司 | Nanometer titania modified loading method and application |
| CN106587691A (en) * | 2016-10-28 | 2017-04-26 | 同济大学 | Method for preparing modified micro particles coated with graphene oxide |
| CN107142780A (en) * | 2017-05-15 | 2017-09-08 | 柳州博泽科技有限公司 | A kind of surface treatment method of nano titanium oxide applied to facing paper |
| CN110342900A (en) * | 2018-04-08 | 2019-10-18 | 江苏未名之光纳米科技有限公司 | A kind of height heat-barrier material and preparation method thereof |
| CN109759040A (en) * | 2019-03-05 | 2019-05-17 | 辽宁石油化工大学 | A kind of preparation method of modifying titanium dioxide |
| CN111607446A (en) * | 2020-06-30 | 2020-09-01 | 国网河南省电力公司新野县供电公司 | High-insulation high-stability modified transformer oil |
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| CN112603838A (en) * | 2020-11-30 | 2021-04-06 | 上海蔻沣生物科技有限公司 | Nano titanium dioxide slurry oil and preparation method and application thereof |
| CN112981501A (en) * | 2021-03-05 | 2021-06-18 | 赵琳琳 | Composite bright nickel plating solution |
| CN112981501B (en) * | 2021-03-05 | 2024-03-01 | 惠州市荣安达化工有限公司 | Composite bright nickel plating solution |
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| CN114011476A (en) * | 2021-11-08 | 2022-02-08 | 四川大学 | Adsorption-catalytic decomposition integrated titanium dioxide and application thereof |
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Application publication date: 20120912 |