CN102674737A - Special external reactant for self-cleaning concrete and preparation method thereof - Google Patents
Special external reactant for self-cleaning concrete and preparation method thereof Download PDFInfo
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- CN102674737A CN102674737A CN2012101843180A CN201210184318A CN102674737A CN 102674737 A CN102674737 A CN 102674737A CN 2012101843180 A CN2012101843180 A CN 2012101843180A CN 201210184318 A CN201210184318 A CN 201210184318A CN 102674737 A CN102674737 A CN 102674737A
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Abstract
The invention discloses a special external reactant for self-cleaning concrete and a preparation method thereof. The external reactant comprises the following ingredients in percentage by weight: 3-10% of Fe-doped nano titanium dioxide powder, 0.3-0.8% of surfactant and 89.5-96.5% of dispersant. The preparation method comprises the following steps of: firstly preparing the Fe-doped nano titanium dioxide powder with the average particle diameter of 60nm by a spontaneous combustion method; and then dispersing the obtained powder in a liquid phase so as to prepare the special external reactant for the self-cleaning concrete. The special external reactant disclosed by the invention has the following advantages that Fe<3+> solid is dissolved in a nano titanium dioxide system by utilizing a spontaneous combustion technology, so that the absorption threshold of a photocatalysis material is improved, and the solar energy utilization ratio is improved; and the nano powder is uniformly dispersed in a liquid phase system through the surfactant, so that the nano powder can be uniformly dispersed to a concrete system.
Description
Technical field
The present invention relates to building material field, particularly a kind of automatically cleaning concrete special additive and preparation method thereof.
Background technology
Along with the fast development of cement concrete technology, developed concrete abroad with self-cleaning function.Mixed in this concrete and had the nano titanium oxide of photocatalysis.Through the photocatalysis of nano titanium oxide, decompose the dirt of concrete surface, dirt is reduced at the sticking power of concrete surface, be easy to by rainwater and gasflow clean-up, therefore can keep the cleaning of concrete surface; Can also decompose simultaneously the waste gas that the vehicles such as carbon monoxide, nitrogen peroxide and other oxynitride and factory discharge, thereby this concrete also has the effect that purifies air.
In this kind concrete adulterated nano titanium oxide have that spectrochemical property is stable, catalytic efficiency (is high, oxidation capacity is strong, advantage such as nontoxic, inexpensive, non-secondary pollution.But because absorbing threshold value, it is 387nm, lower to solar energy utilization rate, because the recombination rate in light induced electron and hole is high, causes quantum yield low, thereby greatly reduce catalytic activity in addition.In addition, because the surfactivity of nanoparticle is higher, be highly susceptible to reuniting, directly add in the concrete with the powder form, under the mechanical force of stirrer, nano-powder is difficult to homodisperse in concrete system.
Summary of the invention
Goal of the invention: to the deficiency of above-mentioned prior art; The object of the present invention is to provide a kind of concrete special additive of automatically cleaning and preparation method thereof that is used to prepare; Improve the absorption threshold value of photocatalyst material through the Fe doping; Expansion is dispersed in the liquid-phase system nano-powder to solar energy utilization rate through tensio-active agent uniformly, and nano-powder is distributed in the concrete system uniformly.
Technical scheme: for solving the problems of the technologies described above; The technical scheme that the present invention adopted is: a kind of automatically cleaning concrete special additive; Comprise following components in weight percentage: Fe doped nano titanium dioxide powder 3-10%, tensio-active agent 0.3-0.8%, dispersion agent 89.5-96.5%.
Among the present invention, said Fe doped nano titanium dioxide powder is to be the Fe doped nano titanium dioxide powder of 60nm by the median size that auto-combustion method prepares.
Among the present invention, said tensio-active agent is one or more in Hydrocerol A, oleic acid, the Triple Pressed Stearic Acid.It act as the surface of clad nano particle, reduces the surface energy of nanoparticle, makes it stable existence in dispersion system.
Among the present invention, said dispersion agent is any of methyl alcohol, ethanol and Virahol.
The preparation method of above-mentioned automatically cleaning concrete special additive, this method comprises the steps:
(1) auto-combustion method prepares the Fe doped nano titanium dioxide powder that median size is 60nm;
(2) Fe doped nano titanium dioxide powder is placed dispersion agent, ultra-sonic dispersion, the back of waiting to be uniformly dispersed adds tensio-active agent, promptly gets automatically cleaning concrete special additive.
As preparing method's among the present invention further improvement, the concrete operations step of step (1) is following:
11) preparation Titanium Nitrate solution: it is in 40% the hydrofluoric acid that white titanium pigment is dissolved in mass concentration; Obtain titanium tetrafluoride solution; The adding mass concentration is 25% strong aqua generation titanium hydroxide deposition in solution; Repeatedly during repeatedly to the pH=7 of filtrating, resolution of precipitate in mass concentration is 65% concentrated nitric acid, is obtained Titanium Nitrate solution with deionized water wash in the back with deionized water wash;
12) with mass ratio be iron nitrate and the Titanium Nitrate mixed dissolution of 1:25; Add a certain amount of Hydrocerol A and an ammonium nitrate in the Titanium Nitrate solution that in step 11), obtains then; Regulate pH value to 6 with ammoniacal liquor; In 80 ℃ of water-baths, constantly stir until forming gel, then dry 12 hours formation xerogel in 80 ℃ of baking ovens; The mole number of Hydrocerol A equates that with the total mole number of metals ion the consumption of an ammonium nitrate is 1/4 amount of Hydrocerol A, and wherein metals ion is iron ion and a titanium ion contained in the Fe doped nano titanium dioxide powder.
13) xerogel is placed crucible, on electric furnace, add the thermal initiation auto-combustion, form dendritic fluffy product, obtain the Fe doped nano titanium dioxide powder of 60nm after product is ground.
Preferably, said Titanium Nitrate is for handling the solution that white titanium pigment obtains through hydrofluoric acid, strong aqua, concentrated nitric acid, and Titanium Nitrate is the precursor that auto-combustion prepares nano titanium oxide.
Preferably, said iron nitrate is analytically pure chemical reagent.Iron nitrate is that auto-combustion prepares the Fe doped nano titanium dioxide dopant ion Fe is provided
3+
Preferably, said Hydrocerol A is analytically pure chemical reagent, and Hydrocerol A is iron ion and titanium ion homodisperse sequestrant in gel, and provides auto-combustion needed fuel.
Preferably, said an ammonium nitrate and ammoniacal liquor are analytically pure chemical reagent, its again acting as in the system needed oxygenant of auto-combustion and regulation system pH value are provided.
Beneficial effect: compared with prior art, advantage of the present invention is: through the sequestering action and the auto-combustion reaction of Hydrocerol A, with dopant ion Fe
3+Be solid-solubilized in Fe in the titanium oxide lattice uniformly
3+Doping promoted light induced electron to separate effectively with the hole, suppress that it is compound, improve photocatalytic activity.And can bring up to about 490nm absorbing threshold value, can greatly improve utilising efficiency to sun power.Through the synergy of tensio-active agent and dispersion agent, the nanometer that makes stable existence is analyzed dispersion system, and can make the finely dispersed automatically cleaning concrete of nano-powder.
Embodiment
Through concrete embodiment the present invention is further specified below; Should be pointed out that for the person of ordinary skill of the art, under the prerequisite that does not break away from the principle of the invention; Can also make some modification and improvement, these also should be regarded as belonging to protection scope of the present invention.
Embodiment 1: a kind of automatically cleaning concrete special additive comprises following components in weight percentage: Fe doped nano titanium dioxide powder 3%, and tensio-active agent 0.5%, dispersion agent 96.5%, wherein, tensio-active agent is a Hydrocerol A; Dispersion agent is a methyl alcohol.
The preparation method of above-mentioned automatically cleaning concrete special additive is following:
The first step, preparation Fe doped nano titanium dioxide powder is specially:
At first; Preparation Titanium Nitrate solution: it is in 40% the hydrofluoric acid that analytically pure white titanium pigment is dissolved in analytically pure mass concentration; Obtain titanium tetrafluoride solution, in titanium tetrafluoride solution, add analytically pure mass concentration again and be 25% strong aqua and generate the titanium hydroxide deposition, with deionized water wash repeatedly the back with deionized water wash during repeatedly to the pH=7 of filtrating; Resolution of precipitate in analytically pure mass concentration is 65% concentrated nitric acid, is obtained Titanium Nitrate solution;
Secondly; With mass ratio is iron nitrate and the Titanium Nitrate mixed dissolution of 1:25; In solution, add a certain amount of analytically pure Hydrocerol A and analytically pure an ammonium nitrate then; Regulate pH value to 6 with ammoniacal liquor, in 80 ℃ of water-baths, constantly stir until forming gel, drying formed xerogel in 12 hours in 80 ℃ of baking ovens then; The mole number of Hydrocerol A equates that with the total mole number of metals ion the consumption of an ammonium nitrate is 1/4 amount of Hydrocerol A, and wherein metals ion is iron ion and a titanium ion contained in the Fe doped nano titanium dioxide powder.
At last, xerogel is placed crucible, on electric furnace, add the thermal initiation auto-combustion, form dendritic fluffy product, obtain the Fe doped nano titanium dioxide powder of 60nm after product is ground.
In second step, it is 96.5.5% methyl alcohol that the Fe doped nano titanium dioxide powder of 60nm is placed mass percent, ultra-sonic dispersion, and it is 0.5% Hydrocerol A that the back of waiting to be uniformly dispersed adds mass percent, promptly gets automatically cleaning concrete special additive.
Embodiment 2: basic identical with embodiment 1, different is the component of automatically cleaning concrete special additive, is specially: Fe doped nano titanium dioxide powder 4%, and tensio-active agent 0.6%, dispersion agent 95.4%, wherein, tensio-active agent is a Triple Pressed Stearic Acid; Dispersion agent is a methyl alcohol.
Embodiment 3: basic identical with embodiment 1, different is the component of automatically cleaning concrete special additive, is specially: Fe doped nano titanium dioxide powder 3.5%, and tensio-active agent 0.5%, dispersion agent 96%, wherein, tensio-active agent is a Hydrocerol A; Dispersion agent is a methyl alcohol.
By embodiment 1 to 3 prepared automatically cleaning concrete special additive; Measure its automatically cleaning concrete stable and that prepare that absorbs threshold value and dispersion system effect (it is 5% glucose solution that the concrete test block for preparing is put into 30 ℃ of concentration, makes an experiment under the illumination condition) of keeping a public place clean.The concrete experiments of each embodiment, in same raw materials, technical indicator (comparing) as shown in the table under the situation of identical proportioning with normal concrete and the titanium doped concrete of nanometer titanium dioxide:
| Embodiment | 1 | 2 | 3 | Nano titanium oxide | Normal concrete |
| Absorb threshold value (nm) | 495 | 495 | 495 | 387 | / |
| Dispersed system stability | 7d precipitates fully | 7d precipitates fully | 6d precipitates fully | 12h precipitates fully | / |
| The redispersion performance | Well | Well | Well | Well | / |
| The effect of keeping a public place clean | Do not grow mikrobe, cleaning | Do not grow mikrobe, cleaning | Do not grow mikrobe, cleaning | Do not grow mikrobe, cleaning | The 2d surface grows mould |
From the table can find out, use this special additive after, concrete oneself keeps a public place clean functional.And for nano silica powder, the absorption threshold value of the stability of dispersed system and nano-powder all has significantly to be improved.
Embodiment 4: basic identical with embodiment 1, different is the component of automatically cleaning concrete special additive, is specially: Fe doped nano titanium dioxide powder 3%, Triple Pressed Stearic Acid 0.2%, oleic acid 0.3%, ethanol 96.5%.
Embodiment 5: basic identical with embodiment 1, different is the component of automatically cleaning concrete special additive, is specially: Fe doped nano titanium dioxide powder 10%, Triple Pressed Stearic Acid 0.5%, Virahol 89.5%.
Embodiment 6: basic identical with embodiment 1, different is the component of automatically cleaning concrete special additive, is specially: Fe doped nano titanium dioxide powder 6%, oleic acid 0.8%, ethanol 93.2%.
Embodiment 7: basic identical with embodiment 1, different is the component of automatically cleaning concrete special additive, is specially: Fe doped nano titanium dioxide powder 6%, Hydrocerol A 0.2%, oleic acid 0.5%, Triple Pressed Stearic Acid 0.1%, ethanol 93.2%.
Embodiment 8: basic identical with embodiment 1, different is the component of automatically cleaning concrete special additive, is specially: Fe doped nano titanium dioxide powder 10%, Hydrocerol A 0.2%, oleic acid 0.3%, ethanol 89.5%.
Embodiment 9: basic identical with embodiment 1, different is the component of automatically cleaning concrete special additive, is specially: Fe doped nano titanium dioxide powder 3.5%, Triple Pressed Stearic Acid 0.2%, Hydrocerol A 0.6%, alcohol 95 .7%.
Claims (10)
1. an automatically cleaning concrete special additive is characterized in that, comprises following components in weight percentage: Fe doped nano titanium dioxide powder 3-10%, tensio-active agent 0.3-0.8%, dispersion agent 89.5-96.5%.
2. automatically cleaning concrete special additive according to claim 1 is characterized in that: said Fe doped nano titanium dioxide powder is to be the Fe doped nano titanium dioxide powder of 60nm by the median size that auto-combustion method prepares.
3. automatically cleaning concrete special additive according to claim 1 is characterized in that: said tensio-active agent is one or more in Hydrocerol A, oleic acid, the Triple Pressed Stearic Acid.
4. automatically cleaning concrete special additive according to claim 1 is characterized in that: said dispersion agent is any of methyl alcohol, ethanol and Virahol.
5. according to the preparation method of each said automatically cleaning concrete special additive in the claim 1 to 4, it is characterized in that this method comprises the steps:
(1) auto-combustion method prepares the Fe doped nano titanium dioxide powder that median size is 60nm;
(2) Fe doped nano titanium dioxide powder is placed dispersion agent, ultra-sonic dispersion, the back of waiting to be uniformly dispersed adds tensio-active agent, promptly gets automatically cleaning concrete special additive.
6. according to the preparation method of the said automatically cleaning concrete of claim 5 special additive, it is characterized in that the concrete operations step of step (1) is following:
11) preparation Titanium Nitrate solution: it is in 40% the hydrofluoric acid that white titanium pigment is dissolved in mass concentration; Obtain titanium tetrafluoride solution; The adding mass concentration is 25% strong aqua generation titanium hydroxide deposition in solution; When using deionized water wash repeatedly to the pH=7 of filtrating with resolution of precipitate in mass concentration is 65% concentrated nitric acid, obtain Titanium Nitrate solution;
12) with mass ratio be iron nitrate and the Titanium Nitrate mixed dissolution of 1:25; Add a certain amount of Hydrocerol A and an ammonium nitrate in the Titanium Nitrate solution that in step 11), obtains then; Regulate pH value to 6 with ammoniacal liquor; In 80 ℃ of water-baths, constantly stir until forming gel, then dry 12 hours formation xerogel in 80 ℃ of baking ovens;
13) xerogel is placed crucible, on electric furnace, add the thermal initiation auto-combustion, form dendritic fluffy product, obtain the Fe doped nano titanium dioxide powder of 60nm after product is ground.
7. according to the preparation method of the said automatically cleaning concrete of claim 6 special additive, it is characterized in that said white titanium pigment is analytically pure chemical reagent.
8. the preparation method of automatically cleaning concrete special additive according to claim 6 is characterized in that: said iron nitrate is analytically pure chemical reagent.
9. the preparation method of automatically cleaning concrete special additive according to claim 6 is characterized in that: said Hydrocerol A is analytically pure chemical reagent.
10. the preparation method of automatically cleaning concrete special additive according to claim 6 is characterized in that: said an ammonium nitrate and ammoniacal liquor are analytically pure chemical reagent.
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| CN102674737B CN102674737B (en) | 2014-06-18 |
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| CN107176820A (en) * | 2017-06-22 | 2017-09-19 | 盐城工学院 | A kind of concrete of durability concrete photocatalysis slurry and removable NOx |
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| CN107176820A (en) * | 2017-06-22 | 2017-09-19 | 盐城工学院 | A kind of concrete of durability concrete photocatalysis slurry and removable NOx |
| CN107176820B (en) * | 2017-06-22 | 2019-08-06 | 盐城工学院 | A kind of concrete of durability concrete photocatalysis slurry and removable NOx |
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