CN103525134A - Surface modification method of nano-titanium dioxide - Google Patents
Surface modification method of nano-titanium dioxide Download PDFInfo
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- CN103525134A CN103525134A CN201310438733.9A CN201310438733A CN103525134A CN 103525134 A CN103525134 A CN 103525134A CN 201310438733 A CN201310438733 A CN 201310438733A CN 103525134 A CN103525134 A CN 103525134A
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Abstract
The invention relates to a modification method of nano-titanium dioxide. The modification method comprises the steps of (1) adding nano-titanium dioxide powder into an ethanol solution, and performing ultrasonic vibration to uniformly mix the nano-titanium dioxide powder in the ethanol solution to obtain the ethanol solution of the nano-titanium dioxide; (2) adding a silane coupling agent KH-570 into a mixed solution of ethanol and deionized water, and performing ultrasonic vibration to hydrolyze the silane coupling agent KH-570 in the mixed solution; (3) adding the mixed solution after hydrolysis, which is obtained in the step (2), into the ethanol solution obtained in the step (1), performing ultrasonic vibration, and then stirring for reacting at the temperature of 70-90 DEG C; performing suction filtration, washing, drying and grinding to obtain the surface modified nano-titanium dioxide. The dispersity of the nano-titanium dioxide modified by the silane coupling agent KH-570 is improved, so that the weatherability, the ultraviolet resistance and the like are improved. The modification method provided by the invention has the advantages of low price of raw materials, simple process and low cost, and is favorable for industrial production.
Description
Technical field
The invention belongs to nanometer titanic oxide material field, particularly a kind of surface modification method of nano titanium oxide.
Background technology
Due to nano titanium oxide, there is the features such as good anti-ultraviolet property, weather resisteant, chemical resistance, thermotolerance, photocatalytic, thermostability, be widely used in the industries such as pigment, rubber, plastics, papermaking, also as photocatalyst, photoelectric cell, ultraviolet screening agent etc., be widely used simultaneously.Not surface treated nano titanium oxide surface can be higher, and surface contains polar group hydroxyl, so nano titanium oxide is easily because polar adsorption or moisture absorption produce reunion, becomes the larger-size coacervate with some weak linkage interfaces.The nano titanium oxide of surface modification does not join while preparing matrix material in high molecular polymer as additive, usually exist nanoparticle to disperse inhomogeneous problem, thereby make the over-all properties of its nano composite material of preparing poor, in application, be limited by very large.Therefore nano titanium oxide being carried out to finishing, is to improve its dispersiveness in high molecular polymer matrix, brings into play its functional performance, prepares the essential precondition of functional type nano composite material.
Existing patent of invention " a kind of method of modifying of nano titanium oxide " (publication number: be CN102660153A), by chemical reaction, coupling agent KH-550 is grafted on to nano titanium oxide surface, thereby realize the surface modification to nano titanium oxide.Existing patent of invention " a kind of surface treatment method of nano titanium oxide " (publication number: CN1982349A) carry out surface aggregate with butyl (tetra) titanate to nano titanium oxide surface preparation with methyl methacrylate, make titanium dioxide nanoparticle surface form one layer of polymeric film.Existing patent of invention " a kind of method of silane coupler modified nano titanic oxide sol " (publication number: CN102031022A) with the mixing solutions of ethanol and water and add hydrochloric acid to react with butyl (tetra) titanate to generate nano titanic oxide sol, add again the rear coupling agent kh-570 of hydrolysis and nano titanium oxide surface hydroxyl generation condensation reaction, make coupling agent modified nano titanic oxide sol.
Three above-mentioned invention disclosed patents are all to a certain degree improving the dispersiveness of nano titanium oxide in organic medium.But their surface-treated technique is more complicated, control process difficulty, cost is higher.This is just simple in the urgent need to inventing a kind of technique, the method for the surface-modified nano titanium dioxide of easy handling.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of surface modification method of nano titanium oxide, and the method has solved the agglomeration traits of titanium dioxide nanoparticle, improves its dispersiveness, weather resisteant, anti-ultraviolet property.
The method of modifying of a kind of nano titanium oxide of the present invention, comprising:
(1) nano titanium dioxide powder is added in ethanolic soln, sonic oscillation mixes nano titanium dioxide powder in ethanolic soln, obtains the ethanolic soln of nano titanium oxide;
(2) Silane coupling reagent KH-570 is joined in the mixing solutions of ethanol and deionized water, ultra-sonic oscillation are hydrolyzed Silane coupling reagent KH-570 in mixing solutions;
(3) mixed solution after the hydrolysis of step (2) gained is joined to ultra-sonic oscillation 0.1-2 hour, then stirring reaction 0.5-5h at 70-90 ℃ in the ethanolic soln of step (1) gained; Reaction finishes rear suction filtration, washing, oven dry, grinding, obtains the nano titanium oxide of surface modification.
The mass concentration of the ethanolic soln of the nano titanium oxide described in step (1) is 5%.
The consumption of the Silane coupling reagent KH-570 described in step (2) is the 1-3% of nano titanium oxide quality.
In the mixing solutions of the ethanol described in step (2) and deionized water, the volume ratio of ethanol and deionized water is 20:1.
The time of the ultra-sonic oscillation described in step (3) is 0.5h.
The temperature of the reaction described in step (3) is 80 ℃, and the time is 2h.
Present method relates to a kind of nano titanium oxide surface modification method, mainly to react by nano titanium oxide surface hydroxyl and coupling agent, coupling agent is grafted on nano titanium oxide surface, thereby dispersiveness, weathering resistance and the automatically cleaning character of improving nano titanium oxide, belong to powdered material processing technique field.
The reaction process of Silane coupling reagent KH-570 modified nano-titanium dioxide is as Fig. 1; This reaction process is divided into three steps, and the first step is that 3 hydrolysising groups that are connected with Si in KH-570 react with water, generates silanol; Second step is the oligosiloxane that between silanol, dehydrating condensation becomes Si-OH; The 3rd step is that the Si-OH of oligosiloxane reacts with the OH on nano titanium oxide, produces dehydration and solidify in the process of heating, reaches with nano-titanium dioxide powder and forms firmly covalent bonds.
(1) FT-IR analyzes
Fig. 2 is respectively the nano titanium oxide (a) of not finishing and the nano titanium oxide (b) of finishing and coupling agent kh-570 (c) infrared spectrum, as can be seen from Figure, with spectrogram (a) contrast of pure nano titanium oxide, the infrared spectrum (b) of modification nano titanium oxide later occurs significantly to change.Nano titanium oxide after modification is at 2917cm
-1, 2847cm
-1, 1726cm
-1, 1626cm
-1, 1467cm
-1there is obvious charateristic avsorption band, 2917cm in these characteristic peaks
-1, 2847cm
-1the stretching vibration peak of C-H key on corresponding coupling agent, 1726cm
-1the peak correspondence at place the stretching vibration peak of coupling agent C=O key, 1626cm
-1the peak correspondence at place the stretching vibration peak of coupling agent C=C key, 1467cm
-1the peak correspondence at place on coupling agent the flexural vibration peak of C-H key in methylene radical.Show based on the above results: coupling agent kh-570 and TiO
2the coupling of hydroxyl phase or the link of nanoparticle surface, be combined in nano-titania particle surface with the form of chemical bond.
(2) tem observation
Nano titanium dioxide powder before and after finishing is scattered in dehydrated alcohol, with the pattern of transmission electron microscope observation nanoparticle; In Fig. 3, (A) is the TEM figure of not surface finish nano titanium dioxide, is (B) the TEM figure of Silane coupling reagent KH-570 surface finish nano titanium dioxide; From A figure, can find out that dash area is darker in the drawings without coupling agent modified nano titanium oxide, and in figure, most of nano-titania particle pattern is difficult to discrimination, nano-titania particle reunion is described together, bad dispersibility.Dash area is lighter in the drawings from B figure, can to see after coupling agent modified nano titanium oxide, and in figure, most of nano-titania particle pattern can go out in discrimination.Explanation after coupling agent graft modification between nanoparticle interaction force weaken, be not easy to reunite, improved the dispersiveness of nanoparticle.
Comprehensive above situation, this patent the key technical indexes is practical, rationally reliable, this patent advantage is that technique is simple, easy handling, reduces costs, and has realized coupling agent kh-570 and has successfully been grafted on nano titanium oxide surface, thereby reach the object of finishing, the dispersiveness of the nano titanium oxide after finishing in organic medium be improved significantly.
Beneficial effect:
(1) dispersiveness of the nano titanium oxide of Silane coupling reagent KH-570 modification is improved, thereby improves its weathering resistance and anti-ultraviolet property etc.;
(2) raw material valency of the present invention is low, and technique is simple, cost is low, is beneficial to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of coupling agent kh-570 surface finish nano titanium dioxide process
Y is
it is non-hydrolysising group; X is-OCH
3, be hydrolysable group;
Fig. 2 is that Fourier transformation infrared spectrometer records Silane coupling reagent KH-570 surface finish nano titanium dioxide infrared spectrogram; (a) nano titanium oxide of finishing not; (b) nano titanium oxide of coupling agent finishing; (c) Silane coupling reagent KH-570; English in Fig. 2 is revised as to corresponding Chinese.
Fig. 3 is the shape appearance figure with transmission electron microscope observation nanoparticle; (A) being the TEM figure of not surface finish nano titanium dioxide, is (B) the TEM figure of silane resin acceptor kh-550 surface finish nano titanium dioxide.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
(1) nano titanium dioxide powder is joined in ethanolic soln, being configured to mass concentration is 5% ethanolic soln, and sonic oscillation mixes nano titanium dioxide powder in ethanolic soln;
(2) press 1% of titanium dioxide quality, get in the mixing solutions that Silane coupling reagent KH-570 adds ethanol and deionized water, the volume ratio of ethanol and deionized water is 20:1, be configured to mass concentration and be 1% mixing solutions, ultra-sonic oscillation are hydrolyzed Silane coupling reagent KH-570 in alcohol water mixed solution;
(3) mixing solutions of step B gained is added in the ethanolic soln of steps A gained to ultra-sonic oscillation half an hour, then stirring reaction 2h at 80 ℃ of water-baths; Gained mixing solutions suction filtration, washing, oven dry, grinding, obtain the nanometer titanium dioxide titanium products of surface modification.
Embodiment 2
(1) nano titanium dioxide powder is joined in ethanolic soln, being configured to mass concentration is 5% ethanolic soln, and sonic oscillation mixes nano titanium dioxide powder in ethanolic soln;
(2) press 3% of titanium dioxide quality, get in the mixing solutions that Silane coupling reagent KH-570 adds ethanol and deionized water, the volume ratio of ethanol and deionized water is 20:1, be configured to mass concentration and be 3% mixing solutions, ultra-sonic oscillation are hydrolyzed Silane coupling reagent KH-570 in alcohol water mixed solution;
(3) mixing solutions of step B gained is added in the ethanolic soln of steps A gained to ultra-sonic oscillation half an hour, then stirring reaction 2h at 80 ℃ of water-baths; Gained mixing solutions suction filtration, washing, oven dry, grinding, obtain the nanometer titanium dioxide titanium products of surface modification.
(1) nano titanium dioxide powder is joined in ethanolic soln, being configured to mass concentration is 5% ethanolic soln, and sonic oscillation mixes nano titanium dioxide powder in ethanolic soln;
(2) press 5% of titanium dioxide quality, get in the mixing solutions that Silane coupling reagent KH-570 adds ethanol and deionized water, the volume ratio of ethanol and deionized water is 20:1, be configured to mass concentration and be 5% mixing solutions, ultra-sonic oscillation are hydrolyzed Silane coupling reagent KH-570 in alcohol water mixed solution;
(3) mixing solutions of step B gained is added in the ethanolic soln of steps A gained to ultra-sonic oscillation half an hour, then stirring reaction 2h at 80 ℃ of water-baths; Gained mixing solutions suction filtration, washing, oven dry, grinding, obtain the nanometer titanium dioxide titanium products of surface modification.
Claims (6)
1. a method of modifying for nano titanium oxide, comprising:
(1) nano titanium dioxide powder is added in ethanolic soln, sonic oscillation mixes nano titanium dioxide powder in ethanolic soln, obtains the ethanolic soln of nano titanium oxide;
(2) Silane coupling reagent KH-570 is joined in the mixing solutions of ethanol and deionized water, ultra-sonic oscillation are hydrolyzed Silane coupling reagent KH-570 in mixing solutions;
(3) mixed solution after the hydrolysis of step (2) gained is joined to ultra-sonic oscillation 0.1-2 hour, then stirring reaction 0.5-5h at 70-90 ℃ in the ethanolic soln of step (1) gained; Reaction finishes rear suction filtration, washing, oven dry, grinding, obtains the nano titanium oxide of surface modification.
2. the method for modifying of a kind of nano titanium oxide according to claim 1, is characterized in that: the mass concentration of the ethanolic soln of the nano titanium oxide described in step (1) is 5%.
3. the method for modifying of a kind of nano titanium oxide according to claim 1, is characterized in that: the consumption of the Silane coupling reagent KH-570 described in step (2) is the 1-3% of nano titanium oxide quality.
4. the method for modifying of a kind of nano titanium oxide according to claim 1, is characterized in that: in the mixing solutions of the ethanol described in step (2) and deionized water, the volume ratio of ethanol and deionized water is 20:1.
5. the method for modifying of a kind of nano titanium oxide according to claim 1, is characterized in that: the time of the ultra-sonic oscillation described in step (3) is 0.5h.
6. the method for modifying of a kind of nano titanium oxide according to claim 1, is characterized in that: the temperature of the reaction described in step (3) is 80 ℃, and the time is 2h.
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| CN103910922A (en) * | 2014-04-22 | 2014-07-09 | 中国水产科学研究院东海水产研究所 | Nano-modified high density polyethylene composite material and preparation method thereof |
| CN104371208A (en) * | 2014-12-05 | 2015-02-25 | 成都领航科技股份有限公司 | Master batch of high-transmittance and high-masking diffusion plate, method for manufacturing master batch and method for manufacturing diffusion plate |
| CN105086520A (en) * | 2014-12-09 | 2015-11-25 | 西南石油大学 | Nanometer SiO2 surface controllable modification method |
| CN105478173A (en) * | 2015-11-28 | 2016-04-13 | 韦昱灵 | Air cleaning material and preparation method thereof |
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| CN103910922A (en) * | 2014-04-22 | 2014-07-09 | 中国水产科学研究院东海水产研究所 | Nano-modified high density polyethylene composite material and preparation method thereof |
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| CN105478173A (en) * | 2015-11-28 | 2016-04-13 | 韦昱灵 | Air cleaning material and preparation method thereof |
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| CN105833814B (en) * | 2016-04-27 | 2018-06-05 | 浙江工业大学 | A kind of preparation method and its microreactor of drop self-driving type microreactor |
| CN106189365B (en) * | 2016-07-15 | 2018-06-22 | 深圳大学 | Modified FxMnySn(1-x-y)O2The preparation method of nano-powder and modified aqueous polyurethane emulsion |
| CN106189365A (en) * | 2016-07-15 | 2016-12-07 | 深圳大学 | Modified Fxmnysn(1 x y)o2nano-powder and the preparation method of modified aqueous polyurethane emulsion |
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Application publication date: 20140122 |