CN103897437B - The tunicary titanium dioxide of titanium dioxide coating method, tool and coating - Google Patents
The tunicary titanium dioxide of titanium dioxide coating method, tool and coating Download PDFInfo
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- CN103897437B CN103897437B CN201210591118.7A CN201210591118A CN103897437B CN 103897437 B CN103897437 B CN 103897437B CN 201210591118 A CN201210591118 A CN 201210591118A CN 103897437 B CN103897437 B CN 103897437B
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 322
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 159
- 238000000576 coating method Methods 0.000 title claims abstract description 88
- 239000011248 coating agent Substances 0.000 title claims abstract description 58
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 30
- 150000002899 organoaluminium compounds Chemical class 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000003960 organic solvent Substances 0.000 claims abstract description 18
- 230000007062 hydrolysis Effects 0.000 claims abstract description 12
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 12
- 238000012545 processing Methods 0.000 claims description 16
- 239000006185 dispersion Substances 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000004411 aluminium Substances 0.000 claims description 5
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- 238000003801 milling Methods 0.000 claims description 5
- -1 plumbous subacetate Chemical compound 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- KILURZWTCGSYRE-LNTINUHCSA-K (z)-4-bis[[(z)-4-oxopent-2-en-2-yl]oxy]alumanyloxypent-3-en-2-one Chemical compound CC(=O)\C=C(\C)O[Al](O\C(C)=C/C(C)=O)O\C(C)=C/C(C)=O KILURZWTCGSYRE-LNTINUHCSA-K 0.000 claims description 3
- BMTAFVWTTFSTOG-UHFFFAOYSA-N Butylate Chemical group CCSC(=O)N(CC(C)C)CC(C)C BMTAFVWTTFSTOG-UHFFFAOYSA-N 0.000 claims description 3
- 239000011888 foil Substances 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 2
- 235000010215 titanium dioxide Nutrition 0.000 claims 11
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims 1
- 150000003608 titanium Chemical class 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000004381 surface treatment Methods 0.000 description 14
- 230000008569 process Effects 0.000 description 7
- 239000007791 liquid phase Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 230000002265 prevention Effects 0.000 description 3
- 238000007665 sagging Methods 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- 238000011179 visual inspection Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 150000001399 aluminium compounds Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 238000010504 bond cleavage reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006253 efflorescence Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 125000001905 inorganic group Chemical group 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000002186 photoelectron spectrum Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
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Abstract
The invention discloses titanium dioxide coating process, the tunicary titanium dioxide of tool and coating.Wherein titanium dioxide coating process comprises: utilize organic solvent and water, makes organo-aluminium compound not exclusively hydrolysis occur, to obtain Alumina gel; And titanium dioxide is contacted with this Alumina gel, to obtain the tunicary titanium dioxide of tool.The method operation is simple, production cost is low, the modified titanium prepared can be made to have inorganic coating and organic coated, and its weathering resistance, sticking power, dispersiveness, wettability, mobility is all excellent simultaneously.
Description
Technical field
The present invention relates to chemical field, particularly, relate to titanium dioxide coating method, the tunicary titanium dioxide of tool and comprise the coating of the tunicary titanium dioxide of this tool.
Background technology
Titanium oxide, is also called titanium dioxide, is a kind of white pigment of brilliance, can be widely used in coating, plastics, papermaking, ink, catalyzer and cosmetics of super quality field.But titanium oxide has very strong photochemical activity, very easily the organic medium molecule caused in application system grows prosperity scission of link and degraded, thus produces the phenomenon such as efflorescence, loss of gloss.Based on above reason, people usually carry out surface treatment to titanium oxide, thus develop multiple titanium dioxide coating process.
But the titanium dioxide coating process of present stage still haves much room for improvement.
Summary of the invention
The present invention completes based on the following discovery of contriver:
According to the character of surface treatment agent, the titanium dioxide powder surface treatment method (titanium dioxide coating process) of present stage can be divided into inorganic surface treatment, organic surface treatment and Combined Processing.Wherein, inorganic surface treatment can at titanium dioxide Surface coating one deck inorganic film, organic surface treatment can at titanium dioxide Surface coating one deck organic film, and Combined Processing can deposit inorganic film and organic film from inside to outside successively on titanium dioxide surface, thus make titanium dioxide have inorganic film and organic film simultaneously.
But contriver finds, the titanium dioxide coating process of above-mentioned present stage has following defect respectively:
1, inorganic surface treatment: cumbersome, energy consumption are high, product yield is lower, the titanium dioxide concentration class with inorganic coating obtained is too high, dispersed poor, particularly: a, coating carry out under liquid-phase condition, thus more hydrogen bond can be introduced, thus the gathering of titanium dioxide can be increased, more need afterwards to carry out drying and processing, and this will cause the clustering phenomena of modified titanium more serious; B, further, in order to reduce above-mentioned rendezvous problem, also needing to introduce high energy dispersion step, thus energy consumption and process complexity can be increased, reducing product yield; C, because coating is obtained by collosol and gel or intermediate processing under certain pH value condition, then through repeatedly washing the neutral PH requirement that just can reach product, complex process must be made; D, need to add a lot of adsorbed ion due to coating process, then must through repeatedly washing the ion could removing absorption, such that complex process, cost are higher, product yield is lower, and cause the wasting of resources.
2, organic surface treatment: adopt dry method coating time, organic surface treatment and titanium dioxide granule bonding force poor, easily depart from; When adopting wet method coating, this process is carried out in aqueous phase, and traditional organic surface treatment is generally water insoluble, thus the bonding force of organic surface treatment and titanium dioxide granule is still relatively weak, organic film after coating easily departs from, especially, in oleaginous system organic surface treatment be easily extracted and with divided titanium dioxide from, decentralized is very poor in oleaginous system to make the tunicary titanium dioxide of tool (also can be called " modified titanium ").
3, Combined Processing: although titanium dioxide can be made to have inorganic film and organic film simultaneously, because it has above-mentioned inorganic surface treatment and organic surface treatment process concurrently, then technique is more numerous and diverse, and cost is higher.
The present invention is intended at least to solve one of technical problem existed in prior art.For this reason, one object of the present invention is to propose that a kind of technique is simple, cost is lower and can obtain the titanium dioxide coating method of the modified titanium having inorganic film and organic film concurrently.
According to an aspect of the present invention, the invention provides a kind of titanium dioxide coating method.According to embodiments of the invention, the method comprises: utilize organic solvent and water, makes organo-aluminium compound not exclusively hydrolysis occur, to obtain Alumina gel; And titanium dioxide is contacted with this Alumina gel, to obtain the tunicary titanium dioxide of tool.Contriver is surprised to find, the method operation is simple, material requested equipment is few, cost is low, and can the inorganic and organic two kinds of retes of disposable introducing, namely, utilize titanium dioxide coating method of the present invention, the modified titanium prepared can be made to have inorganic coating and organic coated, thus the weathering resistance of this modified titanium, sticking power, dispersiveness, wettability, mobility are all excellent simultaneously.
According to a further aspect in the invention, present invention also offers the tunicary titanium dioxide of a kind of tool.According to embodiments of the invention, the tunicary titanium dioxide of this tool is obtained by foregoing titanium dioxide coating method of the present invention.Contriver is surprised to find, the tunicary titanium dioxide of tool of the present invention (in this article sometimes also referred to as " modified titanium ") has inorganic coating and organic coated simultaneously, glossiness is good, and weathering resistance, sticking power, dispersiveness, wettability and mobility are all excellent, and production cost is very low.
According to another aspect of the invention, present invention also offers a kind of coating.According to embodiments of the invention, this coating comprises the tunicary titanium dioxide of foregoing tool of the present invention.According to embodiments of the invention, coating gloss of the present invention and decentralized better.
Additional aspect of the present invention and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage will become obvious and easy understand from accompanying drawing below combining to the description of embodiment, wherein:
Fig. 1 shows the schematic flow sheet of titanium dioxide coating method according to an embodiment of the invention;
Fig. 2 shows the clad structure schematic diagram of the tunicary titanium dioxide of tool according to an embodiment of the invention;
Fig. 3 shows in embodiment 1 the XPS detected result figure of the tunicary titanium dioxide of tool of the present invention prepared.
Embodiment
Embodiments of the invention are described below in detail.Being exemplary below by the embodiment be described with reference to the drawings, only for explaining the present invention, and can not limitation of the present invention being interpreted as.
Titanium dioxide coating method
According to an aspect of the present invention, the invention provides a kind of titanium dioxide coating method.According to embodiments of the invention, the method comprises: utilize organic solvent and water, makes organo-aluminium compound not exclusively hydrolysis occur, to obtain Alumina gel; And titanium dioxide is contacted with this Alumina gel, to obtain the tunicary titanium dioxide of tool.Contriver is surprised to find, the method operation is simple, material requested equipment is few, cost is low, and can the inorganic and organic two kinds of retes of disposable introducing, namely, utilize titanium dioxide coating method of the present invention, the modified titanium prepared can be made to have inorganic coating and organic coated, thus the weathering resistance of this modified titanium, sticking power, dispersiveness, wettability, mobility are all excellent simultaneously.
Describe titanium dioxide coating method of the present invention with reference to the accompanying drawings in detail.
According to one embodiment of present invention, with reference to Fig. 1, the method can comprise:
S100: prepare Alumina gel
First, utilize organic solvent and water, make organo-aluminium compound not exclusively hydrolysis occur, to obtain Alumina gel.
In this step, according to stoichiometry, the consumption of water is less than the amount making organo-aluminium compound generation complete hydrolysis, thus can only make part organo-aluminium compound generation hydrolysis obtain inorganic aluminium compound.According to embodiments of the invention, organic solvent and water is utilized to make organo-aluminium compound the mode of not exclusively hydrolysis occur and be not particularly limited.According to one embodiment of present invention, Alumina gel can be obtained through the following steps: first, utilize organic solvent dissolution organo-aluminium compound, to obtain the organic mixture containing this organo-aluminium compound, next, in this organic mixture, add water, to make the organo-aluminium compound comprised in this organic mixture that not exclusively hydrolysis occur, and obtain Alumina gel.Contriver is surprised to find, first organo-aluminium compound is mixed with organic solvent by adopting, then add water to be hydrolyzed the mode of organo-aluminium compound, effectively can control the degree that hydrolysis occurs organoaluminum, and can improve further and contact subsequently through with titanium dioxide, thus realize carrying out coated efficiency to titanium dioxide.
According to embodiments of the invention, the kind of adoptable organo-aluminium compound is not particularly limited, according to one embodiment of present invention, this organo-aluminium compound can for being selected from least one of aluminum isopropylate, aluminum foil stearate, plumbous subacetate and aluminium acetylacetonate, aluminium secondary butylate.According to a preferred embodiment of the present invention, this organo-aluminium compound is aluminum isopropylate.According to some embodiments of the present invention, organic solvent can be ethanol, Virahol, propyl carbinol, benzene or toluene.According to a preferred embodiment of the present invention, this organic solvent is ethanol.Thereby, it is possible to prepare Alumina gel efficiently, thus effectively can improve the efficiency of titanium dioxide coating, and can production cost be reduced.
In addition, utilize organic solvent dissolution organo-aluminium compound, and the actual conditions making this organo-aluminium compound that not exclusively hydrolysis occur is not particularly limited, according to one embodiment of present invention, every 1mol organo-aluminium compound, can use 1 liter of organic solvent.According to another embodiment of the invention, at the temperature of 40 ~ 80 degrees Celsius, this organo-aluminium compound of organic solvent dissolution can be utilized.According to embodiments of the invention, every 1mol organo-aluminium compound, uses no more than 3mol water.According to one embodiment of present invention, every 1mol organo-aluminium compound, can use 2mol water.Contriver is surprised to find, the Alumina gel adopting aforementioned proportion to obtain, and can improve follow-up the performance obtaining having the titanium dioxide of coating further.
S200: titanium dioxide is contacted with Alumina gel
After acquisition Alumina gel, titanium dioxide is contacted with this Alumina gel, to obtain the tunicary titanium dioxide of tool.In this step, by Alumina gel is contacted with titanium dioxide, the surface being simultaneously deposited in titanium dioxide through being hydrolyzed the inorganic aluminium compound obtained and the organo-aluminium compound not occurring to be hydrolyzed contained in Alumina gel can be made, thus coating can be formed on the surface of titanium dioxide.Thus, convenient and simplely effectively the coating simultaneously with inorganic film and organic film character can be formed on titanium dioxide surface.
According to one embodiment of present invention, before titanium dioxide is contacted with Alumina gel, may further include and this titanium dioxide is carried out drying and dispersion treatment successively.Thus the contact of titanium dioxide and Alumina gel can be improved further, and then realize coating efficiently.Wherein, the condition of carrying out oven dry and dispersion treatment is not particularly limited, as long as make titanium dioxide be suitable for contacting with Alumina gel thus realizing coating.According to one embodiment of present invention, drying and processing 30-500min can be carried out at 70-200 DEG C.According to embodiments of the invention, can utilize airflow milling, in room temperature to 120 DEG C, air pressure is carry out dispersion treatment under the condition of 0.4-1.2MPa.According to a preferred embodiment of the present invention, dispersion treatment is carried out under the air pressure of 0.6MPa.Thereby, it is possible to obtain the dry titanium dioxide of fully dispersion, thus efficiency and the product yield of subsequent disposal can be improved.
According to another embodiment of the invention, titanium dioxide can be joined in Alumina gel by spray pattern, to make this titanium dioxide contact with this Alumina gel, thus, titanium dioxide can be made fully to mix with Alumina gel, thus can coating efficiency be improved.According to another embodiment of the invention, can nozzle be utilized, this titanium dioxide is joined in Alumina gel by spray pattern.Wherein, the type of the nozzle that can adopt is not by special restriction, and according to one embodiment of present invention, the diameter of this nozzle can be 5-10mm, and nozzle pressure can be 0.4-1.2MPa.Thereby, it is possible to make the coating layer on titanium dioxide surface more even, fine and close.
According to embodiments of the invention, the weight ratio of titanium dioxide and Alumina gel can be selected according to actual needs.According to one embodiment of present invention, the weight ratio of this titanium dioxide and this Alumina gel can be 100:0.01-10.
In addition, also it should be noted that, titanium dioxide coating method of the present invention does not need to introduce liquid phase, titanium dioxide do not need to be distributed in liquid phase carry out making beating dispersion, do not need to introduce coating by liquid phase process on titanium dioxide surface yet, and titanium dioxide sample surfaces does not need to introduce the liquid phase substance that any meeting impels it to assemble, and just because this titanium dioxide sample is in dry state always, also just without the need to adopting baking step in technique pilot process, thus can while effectively avoiding material to assemble, Simplified flowsheet, minimizing energy consumption; And titanium dioxide coating method of the present invention does not need repeatedly washing step, can Simplified flowsheet, reduce costs; In addition, utilize the tunicary titanium dioxide of tool that titanium dioxide coating method of the present invention prepares, when it is applied in coating, there is excellent sag prevention performance.
The tunicary titanium dioxide of tool and application thereof
According to a further aspect in the invention, present invention also offers the tunicary titanium dioxide of a kind of tool.According to embodiments of the invention, the tunicary titanium dioxide of this tool is obtained by foregoing titanium dioxide coating method of the present invention.
According to some embodiments of the present invention, the tunicary titanium dioxide of tool of the present invention, its coating is Al (OH) (OCH (CH
3)
2)
2or AlOCH (CH
3)
2(OH)
2.Wherein, Fig. 2 shows the clad structure schematic diagram of the tunicary titanium dioxide of tool of the present invention.As shown in Figure 2, the clad structure of the tunicary titanium dioxide of tool of the present invention is from inside to outside followed successively by: titanium dioxide-coating Al (OH) (OCH (CH
3)
2)
2, wherein, this clad structure can be considered as: titanium dioxide-Al (OH)-(OCH (CH
3)
2)
2(from inside to outside), further, inorganic group Al (OH) can be considered as inorganic film, and by organic group (OCH (CH
3)
2)
2be considered as organic film, thus the tunicary titanium dioxide of tool of the present invention has inorganic coating and organic coated simultaneously.
Contriver is surprised to find, the tunicary titanium dioxide of tool of the present invention (in this article sometimes also referred to as " modified titanium ") has inorganic coating and organic coated simultaneously, glossiness is good, and weathering resistance, sticking power, dispersiveness, wettability and mobility are all excellent, and production cost is very low.In addition, according to embodiments of the invention, the tunicary titanium dioxide of tool of the present invention can be widely used in the preparation technology of various coating, plastics, papermaking, ink, makeup etc., thus can improve the dispersiveness of the product prepared, and reduces production cost.It should be noted that, before for the feature and advantage described by titanium dioxide coating method, be also applicable to this titanium dioxide, repeat no more.
According to another aspect of the invention, present invention also offers a kind of coating.According to embodiments of the invention, this coating comprises the tunicary titanium dioxide of foregoing tool of the present invention.According to embodiments of the invention, coating gloss of the present invention and decentralized are better, sag prevention excellent performance.It should be noted that, before for titanium dioxide coating method and obtain the feature and advantage that have described by the titanium dioxide of coating, be also applicable to this coating, repeat no more.
In addition, it should be noted that, titanium dioxide coating process of the present invention, is that present inventor just completes through the work of arduous creative work and optimization.
Below in conjunction with embodiment, the solution of the present invention is made an explanation.It will be understood to those of skill in the art that the following examples only for illustration of the present invention, and should not be considered as limiting scope of the present invention.Unreceipted concrete technology or condition in embodiment, according to the technology described by the document in this area or condition or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can by the conventional products of commercial acquisition.
Embodiment 1:
According to titanium dioxide coating method of the present invention, with reference to Fig. 1, carry out titanium dioxide coating according to following steps:
First, at 80 DEG C, titanium dioxide is carried out drying and processing 300min, to obtain the titanium dioxide through drying and processing;
Then, get the titanium dioxide of 5Kg through drying and processing, utilize airflow milling, in 90 DEG C, air pressure is carried out dispersion treatment 10min under the condition of 1.0MPa, to obtain the titanium dioxide of fully dispersion;
Next, 0.1mol aluminum isopropylate is joined in 100ml ethanolic soln, and dissolve 24h in 60 DEG C of autoclaves, then slowly instill 0.2mol water, so that preparation obtains the Alumina gel of 100ml;
Then, by the Alumina gel of spray pattern by the 100ml of above-mentioned acquisition, join in the titanium dioxide that 5Kg fully disperses, to obtain the tunicary titanium dioxide of tool.
Take a morsel the tunicary titanium dioxide of tool of above-mentioned acquisition, carries out XPS(and XPS respectively) detect, to carry out ultimate analysis and structure detection to the tunicary titanium dioxide of tool of the present invention, the results are shown in Figure 3.
Fig. 3 shows the photoelectron spectrum figure that the above-mentioned tunicary titanium dioxide of tool of the present invention prepared detects through XPS.As shown in Figure 3, its collection of illustrative plates there is Al element in the tunicary titanium dioxide of tool of the present invention, proves that titanium dioxide surface is wrapped by.
Further, the tunicary titanium dioxide of tool of above-mentioned acquisition of taking a morsel carries out hydrophobicity, particularly: the tunicary titanium dioxide of tool of the above-mentioned acquisition that takes a morsel is placed in water, and visual inspection, found that, the tunicary titanium dioxide of this tool floats on water surface completely, cannot incorporate in water, show that the tunicary titanium dioxide of tool of the present invention has obvious hydrophobic property, namely have well organic coated.
Thus, show that the tunicary titanium dioxide of tool of the present invention prepared by the present embodiment has Al (OH) (OCH (CH
3)
2)
2the coating of structure, namely has inorganic coating and organic coated simultaneously.
Embodiment 2:
According to titanium dioxide coating method of the present invention, with reference to Fig. 1, carry out titanium dioxide coating according to following steps:
First, at 150 DEG C, titanium dioxide is carried out drying and processing 200min, to obtain the titanium dioxide through drying and processing;
Then, get the titanium dioxide of 5Kg through drying and processing, utilize airflow milling, in room temperature, air pressure is carried out dispersion treatment 10min under the condition of 1.2MPa, to obtain the titanium dioxide of fully dispersion;
Next, 0.1mol aluminum foil stearate is joined in 100ml benzene, and dissolve 48h in normal temperature high voltage still, then slowly instill 0.1mol water, so that preparation obtains the Alumina gel of 100ml;
Then, by the Alumina gel of spray pattern by the 100ml of above-mentioned acquisition, join in the titanium dioxide that 5Kg fully disperses, to obtain the tunicary titanium dioxide of tool.
The tunicary titanium dioxide of tool of above-mentioned acquisition of taking a morsel is placed in and carries out hydrophobicity, particularly: the tunicary titanium dioxide of tool of the above-mentioned acquisition that takes a morsel is placed in water, and visual inspection, found that, the tunicary titanium dioxide of this tool floats on water surface completely, cannot incorporate in water, show that the tunicary titanium dioxide of tool of the present invention that the present embodiment prepares has obvious hydrophobic property.
Further, detect through XPS and find the tunicary titanium dioxide of above-mentioned tool, its titanium dioxide surface has the mineral membrane of aluminium element.
Thus, show that the tunicary titanium dioxide of tool of the present invention prepared by the present embodiment has Al (OH) (OOC (CH
2)
17cH
3)
2the coating of structure, namely has inorganic coating and organic coated simultaneously.
Embodiment 3:
According to titanium dioxide coating method of the present invention, with reference to Fig. 1, carry out titanium dioxide coating according to following steps:
First, at 130 DEG C, titanium dioxide is carried out drying and processing 200min, to obtain the titanium dioxide through drying and processing;
Then, get the titanium dioxide of 5Kg through drying and processing, utilize airflow milling, in 80 DEG C, air pressure is carried out dispersion treatment 15min under the condition of 0.8MPa, to obtain the titanium dioxide of fully dispersion;
Next, 1mol aluminium acetylacetonate aluminium secondary butylate is joined in 100ml butanol solution, and dissolve 12h in the autoclave of 50 DEG C, then slowly instill 2mol water, so that preparation obtains the Alumina gel of 100ml;
Then, by the Alumina gel of spray pattern by the 100ml of above-mentioned acquisition, join in the titanium dioxide that 5Kg fully disperses, to obtain the tunicary titanium dioxide of tool.
The tunicary titanium dioxide of tool of above-mentioned acquisition of taking a morsel is placed in and carries out hydrophobicity, particularly: the tunicary titanium dioxide of tool of the above-mentioned acquisition that takes a morsel is placed in water, and visual inspection, found that, the tunicary titanium dioxide of this tool 80% floats on water surface, cannot incorporate in water, show that the tunicary titanium dioxide of tool of the present invention that the present embodiment prepares has hydrophobic property.
Further, detect through XPS and find the tunicary titanium dioxide of above-mentioned tool, its titanium dioxide surface has the mineral membrane of aluminium element.
Thus, show that the tunicary titanium dioxide of tool of the present invention prepared by the present embodiment has Al (OH)
2oC (CH
3) CHCOCH
3the coating of structure, namely has inorganic coating and organic coated simultaneously.
Comparative example:
With reference to the method in the number of patent application patent application that is CN200810216444.3 described in embodiment 1, prepare compound modified titanium (i.e. the tunicary titanium dioxide of tool), wherein this compound modified titanium has inorganic coating and organic coated simultaneously.
Embodiment 4:
According to following steps, the tunicary titanium dioxide of the tool utilizing above-described embodiment 1-3 and comparative example to prepare respectively (sometimes also referred to as " titanium dioxide ") preparation coating:
First, according to the proportions mill base of table 1.
Then, by the mill base of above-mentioned acquisition and all the other each components, mix according to the ratio of table 2, cross 400 mesh sieves, obtain coating.
Wherein, the source based on adopted titanium dioxide: embodiment 1-3 and comparative example, by coating called after sample 1,2,3 and the contrast respectively obtained.
Table 1
Table 2
Then, sagging performance test is carried out to each sample and contrast, particularly: vertically placed by each coating without drying treatment (comprising each sample and contrast) after spraying respectively, check sagging situation.As a result, clearly can observe in sample 1,2 and 3 and only have considerably less coating to flow out into strips, flow out length and be respectively 5cm, 2cm, 4cm; And the sagging performance of the contrast coating of comparative example 1 correspondence is obviously poor, it has more coating to flow out into strips, and length is 10cm, is longer than 5cm.
Thus, show that the coating comprising the tunicary titanium dioxide of tool of the present invention has superior sag prevention performance.And then, show the tunicary titanium dioxide superior performance of tool of the present invention.
In the description of this specification sheets, specific features, structure, material or feature that the description of reference term " embodiment ", " some embodiments ", " example ", " concrete example " or " some examples " etc. means to describe in conjunction with this embodiment or example are contained at least one embodiment of the present invention or example.In this manual, identical embodiment or example are not necessarily referred to the schematic representation of above-mentioned term.And the specific features of description, structure, material or feature can combine in an appropriate manner in any one or more embodiment or example.
Although illustrate and describe embodiments of the invention, those having ordinary skill in the art will appreciate that: can carry out multiple change, amendment, replacement and modification to these embodiments when not departing from principle of the present invention and aim, scope of the present invention is by claim and equivalents thereof.
Claims (12)
1. a titanium dioxide coating method, is characterized in that, comprising:
Utilize organic solvent and water, make organo-aluminium compound that not exclusively hydrolysis occur, obtain Alumina gel; And titanium dioxide is contacted with described Alumina gel, obtain the tunicary titanium dioxide of tool,
Wherein,
Described organic solvent is ethanol, Virahol, propyl carbinol, benzene or toluene,
Described organo-aluminium compound is at least one being selected from aluminum isopropylate, aluminum foil stearate, plumbous subacetate, aluminium acetylacetonate and aluminium secondary butylate,
Every 1mol organo-aluminium compound, uses 1 liter of organic solvent, 2mol water,
The weight ratio of described titanium dioxide and described Alumina gel is 100:0.01-10.
2. method according to claim 1, is characterized in that, obtains described Alumina gel through the following steps:
Utilize organo-aluminium compound described in described organic solvent dissolution, obtain the organic mixture containing described organo-aluminium compound; And
In described organic mixture, add water, make described organo-aluminium compound that not exclusively hydrolysis occur, and obtain described Alumina gel.
3. method according to claim 1 and 2, is characterized in that, described organo-aluminium compound is aluminum isopropylate.
4. method according to claim 1 and 2, is characterized in that, described organic solvent is ethanol.
5. method according to claim 2, is characterized in that, at the temperature of 40 ~ 80 degrees Celsius, utilizes organo-aluminium compound described in described organic solvent dissolution.
6. method according to claim 1, is characterized in that, before being contacted with described Alumina gel by described titanium dioxide, comprises further and is carried out successively drying and dispersion treatment by described titanium dioxide.
7. method according to claim 6, is characterized in that, carries out described drying and processing 30-500min at 70-200 DEG C.
8. method according to claim 6, is characterized in that, utilizes airflow milling, and in room temperature to 120 DEG C, air pressure is carry out described dispersion treatment under the condition of 0.4-1.2MPa.
9. method according to claim 1, is characterized in that, is joined in described Alumina gel by described titanium dioxide by spray pattern, to make described titanium dioxide contact with described Alumina gel.
10. method according to claim 9, is characterized in that, utilizes nozzle, joins in described Alumina gel by described titanium dioxide by spray pattern,
Wherein, nozzle pressure is 0.4-1.2MPa, and nozzle diameter is 5-8mm.
11. 1 kinds of tunicary titanium dioxides of tool, it is obtained by the method described in any one of claim 1-10.
12. 1 kinds of coating, is characterized in that, comprise the tunicary titanium dioxide of tool according to claim 11.
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