CN105131656A - Modification method for nanometer titania - Google Patents
Modification method for nanometer titania Download PDFInfo
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Abstract
The invention relates to a modification method for nanometer titania. The method mainly solves the problems that existing titania cannot be stably and evenly dispersed in a polymer matrix and does not have the photocatalytic performance. According to the adopted modification method for nanometer titania, the calcinated nanometer titania and dried 2,2-dimethylolpropionic acid are placed into an alcohol solvent, ultrasonic dispersion processing is performed for 0.5-1.5 h, then, the reaction is continuously performed for 20-30 h at the temperature of 70-90 DEG C under the protection of nitrogen, then solid particles are separated out in a centrifugal machine, the separated particles are dissolved in methyl alcohol or dimethyl formamide again, separation is performed again till a solution is limpid, and the 2,2-dimethylolpropionic acid modification nanometer titania obtained through final separation is placed in a vacuum oven to be dried. According to the technical scheme, the problems are solved, and the method can be used for modification of the nanometer titania.
Description
Technical field
The present invention relates to a kind of nano-titanium dioxide modified method.
Background technology
Nano titanium oxide has anatase titanium dioxide, rutile-type and plate ore deposit type three kinds of crystal formations, and wherein, anatase titanium dioxide photocatalytic is the strongest, rutile-type thermostability and uvioresistant ability best, be all better than amorphous nano titanium oxide.
Because the surface-area/particle diameter ratio of nano particle is very big, very easily reunite in organic polymer, poor compatibility causes dispersed bad, greatly can reduce the performance of nanometer-polymer composites.Therefore the dispersiveness of nano material is the key factor affecting its performance always.The difficulties adding nano titanium oxide in polymeric matrix is how to make nano titanium oxide favorable dispersity, do not gather, and stable dispersion, there is good photocatalysis performance simultaneously.
Do a lot of correlative study how improving the dispersing property of nano material in organic polymer.CN201210128728.3 relates to a kind of method of modifying of nano titanium oxide, mainly introduces functional group on nano-titania particle surface, thus improves the dispersiveness of nano titanium oxide, weathering resistance and self-cleaning property.Wherein a kind of method is broken the nano particle of dispersion reunion, as by supersound process, but this kind of method effect is extremely limited, the interaction between inorganic nanoparticles with organic polymer is with very limited compared with the interaction between inorganic nanoparticles.Another kind method is chemical bonding Graft Method, modification is carried out to nano grain surface, strengthens the interaction between nano particle and polymer chain, reduce the reunion between nano particle, promote the dispersion of nano particle in polymeric matrix, there is good photocatalysis performance simultaneously.Therefore for expanding the use range of nano titanium oxide, efficiently solve nanometer titanium dioxide receive cannot in polymeric matrix stable dispersion, dispersed, and there is the problem of photocatalysis performance, surface modification must be carried out to it.But by the end of at present, not yet there is the method identical with the present invention to complete the surface modification of titanium dioxide nanoparticle.
The present invention solves this problem targetedly.
Summary of the invention
Technical problem to be solved by this invention be in prior art nano titanium oxide cannot in polymeric matrix stable dispersion, dispersed, the problem without photocatalysis performance, a kind of nano-titanium dioxide modified method is newly provided.The method be used for nano-titanium dioxide modified in, have nano titanium oxide can in polymeric matrix stable dispersion, dispersed, the advantage with photocatalysis performance.
For solving the problem, the technical solution used in the present invention is as follows: a kind of nano-titanium dioxide modified method, by the nano titanium oxide and dried 2 after calcining, 2-dimethylol propionic acid is placed in alcoholic solvent, ultrasonic disperse process 0.5 ~ 1.5 hour, then under nitrogen protection, at 70 ~ 90 DEG C, successive reaction is after 20 ~ 30 hours, solid particulate is separated in centrifuges, isolated particle is dissolved into again in methyl alcohol or dimethyl formamide, again be separated, final separation obtain 2, 2-dimethylol propionic acid modified nano-titanium dioxide is placed on drying treatment in vacuum drying oven.
In technique scheme, preferably, described nano titanium oxide is made up of anatase octahedrite and rutile, and the part by weight of anatase octahedrite and rutile is from 10:90 to 90:10.
In technique scheme, preferably, the median size of described nano titanium oxide is between 1 ~ 500nm.
In technique scheme, preferably, described nano titanium oxide is adulterated by transition metal, negatively charged ion, zinc oxide and above-mentioned substance arbitrary combination, and transition metal is any one and combination of iron, chromium, vanadium, nitrogen and cobalt element, and negatively charged ion is any one and combination of nitrogen, sulphur, fluorine anion.
In technique scheme, preferably, described alcoholic solvent includes but not limited to any one of ethanol, Virahol and combines.
In technique scheme, preferably, the weight ratio of described 2,2-dimethylol propionic acids and Virahol is the weight ratio of 0.08 ~ 0.13:1,2,2-dimethylol propionic acid and methyl alcohol is 0.14 ~ 0.19:1.
In technique scheme, preferably, the weight ratio of described 2,2-dimethylol propionic acids and nano titanium oxide is 2 ~ 4:1.
The coordination reaction equation that 2,2-dimethylol propionic acids of the present invention and nano titanium oxide surface occur is as follows:
The present invention can provide a kind of Surface Modification of Nanosized Titanium Dioxide method, effective chemical bond is formed between titanium dioxide nanoparticle and the compound surface containing COOH functional group, other functional groups can polymerization reaction take place, nano titanium oxide stable dispersion, dispersed in polymeric matrix, and there is photocatalysis performance, by the stability in the polymer of modified nano-titanium dioxide obtained by the method and uniformly dispersed all considerably beyond by nano titanium oxide physical blending in polymkeric substance, achieve good technique effect.
Accompanying drawing explanation
Fig. 1 is 2,2-dimethylol propionic acid Electronic Speculum figure before reaction.
Fig. 2 is 2,2-dimethylol propionic acid-n-titanium dioxide Electronic Speculum figure after coordination reaction.
Below by embodiment, the invention will be further elaborated, but be not limited only to the present embodiment.
Embodiment
[embodiment 1]
The preparation method of 2,2-dimethylol propionic acid modified nano-titanium dioxide:
After calcining, by 1g nano titanium oxide (median size is 500nm) and 4g dried 2,2-dimethylol propionic acid (Electronic Speculum as shown in Figure 1) is placed in 45ml Virahol (35.35g), ultrasonic disperse process 1 hour;
Under drying nitrogen protection, successive reaction 24 hours at 80 DEG C;
Solid particulate is separated in centrifuges, then isolated particle is dissolved in 30ml (23.754g) methyl alcohol again, is again separated, until solution is limpid;
Drying treatment in vacuum drying oven is placed on by being finally separated 2, the 2-dimethylol propionic acid modified nano-titanium dioxides obtained.
2,2-dimethylol propionic acid-n-titanium dioxide Electronic Speculum figure after the coordination reaction obtained as shown in Figure 2.
[embodiment 2]
The preparation method of 2,2-dimethylol propionic acid modified nano-titanium dioxide:
After calcining, 2g nano titanium oxide (median size is 300nm) and dried 2, the 2-dimethylol propionic acids of 6g are placed in 60ml Virahol, ultrasonic disperse process 0.5 hour;
Under drying nitrogen protection, successive reaction 30 hours at 70 DEG C;
Solid particulate is separated in centrifuges, then isolated particle is dissolved in 50ml methyl alcohol again, is again separated, until solution is limpid;
Drying treatment in vacuum drying oven is placed on by being finally separated 2, the 2-dimethylol propionic acid modified nano-titanium dioxides obtained.
[embodiment 3]
The preparation method of 2,2-dimethylol propionic acid modified nano-titanium dioxide:
After calcining, 1.5g nano titanium oxide (median size is 500nm) and dried 2, the 2-dimethylol propionic acids of 5g are placed in 50ml Virahol, ultrasonic disperse process 1.5 hours;
Under drying nitrogen protection, successive reaction 20 hours at 90 DEG C;
Solid particulate is separated in centrifuges, then isolated particle is dissolved in 45ml methyl alcohol again, is again separated, until solution is limpid;
Drying treatment in vacuum drying oven is placed on by being finally separated 2, the 2-dimethylol propionic acid modified nano-titanium dioxides obtained.
Claims (7)
1. a nano-titanium dioxide modified method; by the nano titanium oxide and dried 2 after calcining; 2-dimethylol propionic acid is placed in alcoholic solvent; ultrasonic disperse process 0.5 ~ 1.5 hour; then under nitrogen protection; at 70 ~ 90 DEG C, successive reaction is after 20 ~ 30 hours; solid particulate is separated in centrifuges; isolated particle is dissolved into again in methyl alcohol or dimethyl formamide; again be separated; 2, the 2-dimethylol propionic acid modified nano-titanium dioxides that final separation obtains are placed on drying treatment in vacuum drying oven.
2. nano-titanium dioxide modified method according to claim 1, it is characterized in that described nano titanium oxide is made up of anatase octahedrite and rutile, the part by weight of anatase octahedrite and rutile is from 10:90 to 90:10.
3. nano-titanium dioxide modified method according to claim 1, is characterized in that the median size of described nano titanium oxide is between 1 ~ 500nm.
4. nano-titanium dioxide modified method according to claim 1, it is characterized in that described nano titanium oxide is adulterated by transition metal, negatively charged ion, zinc oxide and above-mentioned substance arbitrary combination, transition metal is any one and combination of iron, chromium, vanadium, nitrogen and cobalt element, and negatively charged ion is any one and combination of nitrogen, sulphur, fluorine anion.
5. nano-titanium dioxide modified method according to claim 1, is characterized in that described alcoholic solvent includes but not limited to any one and combination of ethanol, Virahol.
6. nano-titanium dioxide modified method according to claim 1,5, it is characterized in that described 2, the weight ratio of 2-dimethylol propionic acid and alcoholic solvent is the weight ratio of 0.08 ~ 0.13:1,2,2-dimethylol propionic acid and methyl alcohol or dimethyl formamide is 0.14 ~ 0.19:1.
7. nano-titanium dioxide modified method according to claim 1, is characterized in that the weight ratio of described nano titanium oxide and 2,2-dimethylol propionic acid is 2 ~ 4:1.
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| CN106752113A (en) * | 2016-12-14 | 2017-05-31 | 浙江恒逸高新材料有限公司 | A kind of preparation method of modifying titanium dioxide and application |
| CN107320938A (en) * | 2017-08-30 | 2017-11-07 | 河南科技大学 | A kind of portable long jump measurement device |
| CN108084741A (en) * | 2017-11-24 | 2018-05-29 | 合肥紫金钢管股份有限公司 | A kind of steel pipe identifies the preparation process of coding nanometer white pigment before dispatching from the factory |
| CN111253804A (en) * | 2020-04-08 | 2020-06-09 | 齐齐哈尔大学 | Solid painting brush for art design and preparation method thereof |
| CN111346482A (en) * | 2020-03-23 | 2020-06-30 | 薛德 | Low-cost high-efficiency wet flue gas desulfurization and denitrification process |
| CN112359603A (en) * | 2020-12-04 | 2021-02-12 | 长春工业大学 | Water-based hyperbranched polyurethane sizing agent with anti-ultraviolet performance and preparation method thereof |
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| CN107320938A (en) * | 2017-08-30 | 2017-11-07 | 河南科技大学 | A kind of portable long jump measurement device |
| CN108084741A (en) * | 2017-11-24 | 2018-05-29 | 合肥紫金钢管股份有限公司 | A kind of steel pipe identifies the preparation process of coding nanometer white pigment before dispatching from the factory |
| CN108084741B (en) * | 2017-11-24 | 2020-08-07 | 合肥紫金钢管股份有限公司 | Preparation process of nano white pigment for marking and code spraying before leaving factory of steel pipe |
| CN111346482A (en) * | 2020-03-23 | 2020-06-30 | 薛德 | Low-cost high-efficiency wet flue gas desulfurization and denitrification process |
| CN111253804A (en) * | 2020-04-08 | 2020-06-09 | 齐齐哈尔大学 | Solid painting brush for art design and preparation method thereof |
| CN112359603A (en) * | 2020-12-04 | 2021-02-12 | 长春工业大学 | Water-based hyperbranched polyurethane sizing agent with anti-ultraviolet performance and preparation method thereof |
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