CN1067967C - Superfine titanium white surface cladding tech. and reactor thereof - Google Patents
Superfine titanium white surface cladding tech. and reactor thereof Download PDFInfo
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- CN1067967C CN1067967C CN98117967A CN98117967A CN1067967C CN 1067967 C CN1067967 C CN 1067967C CN 98117967 A CN98117967 A CN 98117967A CN 98117967 A CN98117967 A CN 98117967A CN 1067967 C CN1067967 C CN 1067967C
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/10—Coating or impregnating
- C04B20/1055—Coating or impregnating with inorganic materials
- C04B20/1066—Oxides, Hydroxides
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- Inorganic Chemistry (AREA)
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Abstract
The present invention relates to a surface coating technology for ultrafine titanium dioxide and a reaction vessel thereof. In the technology, firstly, dispersing agents are added to titanium dioxide slurry, the titanium dioxide slurry is heated to a certain temperature, sodium silicate is added, the pH value is regulated by diluted sulfuric acid, and heat preservation is carried out; after ageing, a silicon membrane coating process is finished; sodium hydrate is added to regulate the pH value, and then aluminum sulfate is added to regulate the pH value; the product is obtained by filtering, water washing and drying. Nozzles are arranged on two side walls of the reaction vessel, and a feed port and a discharge port are respectively arranged on the upper part and the lower part of the reaction vessel. By using the technology and the reaction vessel of the present invention to coat the surface of titanium dioxide, uniform and compact inorganic membranes can be generated, the thixotropy of the product is lowered, and the chalking resistance and the weatherability are increased.
Description
The present invention relates to a kind of superfine titanium white surface cladding tech and reactor thereof, belong to the material technology field.
The superfine titanic oxide particle grain size is generally 0.2~0.4 μ m.On the one hand, because the particle small specific surface is long-pending big, intergranular cohesive force strengthens, and particle is easily reunited, the dispersed reduction in resin.Therefore, before surface treatment, must make TiO
2The particle of reuniting in the slurries is dispersed into single particle.At present, domestic main dispersing apparatus is a ball mill, and there is following shortcoming in this dispersing method: 1, ball mill is owing to existing back-mixing, so the material particles size-grade distribution that grinds is wide, does not reach monodispersed requirement.2, ball mill is the method for inner dress sand grains mechanical friction, because sand grains and material (TiO
2) contact friction, can bring pollution, reduce TiO
2Purity.3, at present domestic ball mill power consumption is big, the cost height.On the other hand, if TiO
2Particle directly joins in coating, the paint and goes, and then exists weathering resistance poor, and resistance to chalking hangs down and waits detrimentally affect.Therefore; the purpose that inorganic coating is handled is to coat layer protecting film on the surface of titanium dioxide; make and set up barrier together between titanium dioxide surface and the surrounding medium; thereby reduce the photochemical activity of titanium dioxide, help improving dispersiveness, photostabilization, weathering resistance and the resistance to chalking of titanium dioxide.
Existing about TiO in United States Patent (USP) 3437502
2The report of coating method, its coating equipment are common stirring tanks, because the restriction of appointed condition and technology, the coating effect is bad, and coating is inhomogeneous, and independently SiO is arranged
2And Al
2O
3Particle self nucleation, the thixotropy that shows as product in the specific implementation process is big, and sad filter is with dried machine throughput to reduce, and causes every performance index of finished product not reach requirement.
The objective of the invention is to develop a kind of superfine titanium white surface cladding tech and reactor thereof, under the sol-gel theoretical direction, the evenly technology of bag silicon, alclad is proposed, and match with novel high field of turbulent flow coating device, make particle list dispersion process and film process integrated, and making whole technological operation easy, energy consumption is low, and is easy to the engineering amplification.The finished product thixotropy is low, and film forming is even.
The superfine titanium white surface cladding tech of the present invention's development comprises following each step:
(1) be to add dispersion agent Na in 10~30% the titanium dioxide aqueous slurry containing weight percent
2SiO
3, the pH value that makes solution is 8.0~9.0, stir about 15~20 minutes carries out pre-dispersed;
(2) above-mentioned solution is heated to 80 ℃~90 ℃, adds the water glass of 0.1~0.5mol/l, the weight percent that adds water glass is SiO
2: TiO
2=0.01~0.02: 1, be that the pH value of 10~20% dilute sulphuric acid regulator solution is 7.0~8.0 with weight percent, in 80 ℃~90 ℃ insulations 3~4 hours down, ageing;
(3) on the basis of the above-mentioned second step bag silicon fiml, make solution temperature remain on 70 ℃~80 ℃, add 0.1mol/l Tai-Ace S 150, adding the Tai-Ace S 150 stoichiometry is Al
2O
3: TiO
2=0.02~0.04: 1, use 0.1mol/l sodium hydroxide, the pH value of regulator solution is 6~7, stirs 10 minutes;
(4) transferring the pH value of above-mentioned slurries with 0.1mol/l~0.2mol/l Tai-Ace S 150 is 7.0, continues to stir 2~3 hours, filters, be washed to barium salt check sulfate radical-free ion, at last, drying is 4~5 hours under 110 ℃~120 ℃, promptly obtains the superfine titanium white with silicon oxide and aluminum oxide coating.
The present invention has designed the reactor that is specifically designed to the above-mentioned superfine titanium white of preparation, the top of reactor is provided with opening for feed, the bottom is provided with discharge port, on the two side of reactor nozzle is housed, the entrance end of nozzle is taper, and exit end is a cylindricality, and the top opening for feed communicates with the exit end of nozzle, the opening for feed cone angle of nozzle is 13 °~14 °, exit end diameter d and exit end body length L
1Ratio be d: L
1=1: 2.5~3, exit end column length L
1With the long L of entrance end awl
2Ratio be L
1: L
2=1: 2~4.
The cladding process that the present invention proposes coats layer protecting film on the surface of titanium dioxide, makes between the surperficial of titanium dioxide and its medium on every side and sets up barrier together, thereby reduce the photochemical activity of titanium dioxide.Wrap one deck Al again
2O
3Behind the film, form the silicon-aluminium binary coating, and this technology has realized the film forming coating and nucleation look film do not occurred.
The present invention has also designed special-purpose reactor, the reactor content import is designed to form of nozzle,, pressure can be gathered together by the contraction of nozzle endoporus cross section, and be converted into kinetic energy, form with high-speed jet outwards sprays at last, in order to material is disperseed or fragmentation, to generate even, fine and close mineral membrane, and control thickness, reduce the thixotropy of product, easily filter, thereby improved resistance to chalking and the weathering resistance of titanium dioxide in paint greatly.
Description of drawings:
Fig. 1 is the structural representation of the reactor that designs of the present invention.
Fig. 2 (a) and (b), (c), (d) prepare the electromicroscopic photograph of sample for the present invention.
Below in conjunction with accompanying drawing, introduce content of the present invention in detail.
Among Fig. 1, the 1st, reactor, 2 and 5 is nozzles, 3 and 4 is opening for feeds, the 6th, discharge port.
As shown in Figure 1, the present invention has designed the reactor that is specifically designed to the above-mentioned superfine titanium white of preparation, the top of reactor is provided with opening for feed 3 and 4, the bottom is provided with discharge port 6, and nozzle 2 and 5 are housed on the two side of reactor, and the entrance end of nozzle is taper, exit end is a cylindricality, the top opening for feed communicates with the exit end of nozzle, and the opening for feed cone angle of nozzle is 13 °~14 °, exit end diameter d and exit end body length L
1Ratio be d: L
1=1: 2.5~3, exit end column length L
1With the long L of entrance end awl
2Ratio be L
1: L
2=1: 2~4.The mechanism of reactor is to utilize the high field of turbulent flow of nozzle 2 and 5, makes the coating agent can carry out microcosmic fast before film forming and mixes, and produces a uniform concentration distribution, then equably at TiO
2Surface growth.Material TiO
2And H
2From 2,5 pairs of sprays of nozzle, (during bag silicon is Na to membrane-forming agent to O simultaneously with pump
2SiO
3And H
2SO
4, be NaOH and Al during alclad
2(SO
4)
3) enter spray nozzle front end through opening for feed 3,4 respectively and enter reactor together.In impact cavity, mix the back and change aging tank over to, carry out next step work from discharge port 6.
Introduce embodiments of the invention below.
Embodiment 1 adds the dispersion agent water glass in the slurries that contain 15% titanium dioxide, the pH value to 8 of regulator solution, and stirring is carried out pre-dispersed, is heated to 85 ℃, and the stoichiometry of water glass is controlled at SiO
2/ TiO
2=2%, with the pH value to 8 that 10% dilute sulphuric acid is transferred solution, the bag silicon fiml is finished in ageing.On the basis of bag silicon fiml, holding temperature adds the Tai-Ace S 150 of 0.1mol/l and 20% sodium hydroxide simultaneously at 80 ℃, and the stoichiometry of Tai-Ace S 150 is controlled at Al
2O
3/ TiO
2=2%, use the sodium hydroxide adjust pH, maintain pH=8, with the pH to 7.0 of Tai-Ace S 150 adjusting slurry, ageing is washed to no SO
4 2-,, obtain the titanium dioxide of silicon-aluminium binary coating with barium salt check, filtration, 120 ℃ of dryings.The gained sample is even, fine and close film.The TEM photo is seen Fig. 4 (a), surface composition analysis in table l.
Embodiment 2 experimental techniques are with implementing 1.Change the acidity of bag silicon fiml, the pH to 8.5 of regulator solution carries out pre-dispersed, and wraps silicon fiml under this acidity.The gained sample is the loose membrane of sponge shape, and the TEM photo is seen Fig. 4 (b), surface composition analysis in table 1.
Embodiment 4 experimental techniques are with embodiment 1.Change over the consumption of film.SiO
2/ TiO
2=1~1.6%, Al
2O
3/ TiO
2The TEM of=2% gained sample sees Fig. 4 (d), surface composition analysis in table 1.
Claims (2)
1, a kind of superfine titanium white surface cladding tech is characterized in that, this technology comprises following each step:
(1) be to add dispersion agent Na in 10~30% the titanium dioxide aqueous slurry containing weight percent
2SiO
3, the pH value that makes solution is 8.0~9.0, stir about 15~20 minutes carries out pre-dispersed;
(2) above-mentioned solution is heated to 80 ℃~90 ℃, adds the water glass of 0.1~0.5mol/l, the weight percent that adds water glass is SiO
2: TiO
2=0.01~0.02: 1, be that the pH value of 10~20% dilute sulphuric acid regulator solution is 7.0~8.0 with weight percent, in 80 ℃~90 ℃ insulations 3~4 hours down, ageing;
(3) on the basis of the above-mentioned second step bag silicon fiml, make solution temperature remain on 70 ℃~80 ℃, add 0.1mol/l Tai-Ace S 150, add Tai-Ace S 150 weight percent Al
2O
3: TiO
2=0.02~0.04: 1, use 0.1mol/l sodium hydroxide, the pH value of regulator solution is 6~7, stirs 10 minutes;
(4) transferring the pH value of above-mentioned slurries with 0.1mol/l~0.2mol/l Tai-Ace S 150 is 7.0, continues to stir 2~3 hours, filters, be washed to barium salt check sulfate radical-free ion, at last, drying is 4~5 hours under 110 ℃~120 ℃, promptly obtains the superfine titanium white with silicon oxide and aluminum oxide coating.
2, a kind of reactor that is used to prepare above-mentioned superfine titanium white, it is characterized in that, the top of this reactor is provided with opening for feed, the bottom is provided with discharge port, on the two side of reactor nozzle is housed, and the entrance end of nozzle is taper, exit end is a cylindricality, the top opening for feed communicates with the exit end of nozzle, and the opening for feed cone angle of nozzle is 13 °~14 °, exit end diameter d and exit end body length L
1Ratio be d: L
1=1: 2.5~3, exit end column length L
1With the long L of entrance end awl
2Ratio be L
1: L
2=1: 2~4.
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CN98117967A CN1067967C (en) | 1998-09-11 | 1998-09-11 | Superfine titanium white surface cladding tech. and reactor thereof |
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CN98117967A CN1067967C (en) | 1998-09-11 | 1998-09-11 | Superfine titanium white surface cladding tech. and reactor thereof |
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CN1213659A CN1213659A (en) | 1999-04-14 |
CN1067967C true CN1067967C (en) | 2001-07-04 |
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DE10332650A1 (en) * | 2003-07-18 | 2005-02-10 | Kronos International, Inc. | Producing a surface-treated titanium dioxide pigment useful in decorative paper comprises adding aluminum and phosphorus components to an alkaline titanium dioxide suspension and lowering the pH |
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CN100999621B (en) * | 2006-12-20 | 2010-09-01 | 中国科学院山西煤炭化学研究所 | Process for inorganic-organic coating on surface of titanium white powder |
CN100439454C (en) * | 2006-12-20 | 2008-12-03 | 中国科学院山西煤炭化学研究所 | Titanium dioxide surface organic-inorganic modification method |
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US3437502A (en) * | 1968-03-28 | 1969-04-08 | Du Pont | Titanium dioxide pigment coated with silica and alumina |
CN85103475A (en) * | 1985-04-30 | 1986-10-29 | 河南师范大学 | Preparation of rutile type pigment titanium white by high activity crystal |
CN86101534A (en) * | 1986-08-07 | 1988-02-17 | 上海京华化工厂 | The preparation method of water dispersing lide powder pigment |
CN1120978A (en) * | 1994-10-20 | 1996-04-24 | 中国科学院山西煤炭化学研究所 | Method of preparing coated superfine powder with metal surfactant by phase transfer |
-
1998
- 1998-09-11 CN CN98117967A patent/CN1067967C/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3437502A (en) * | 1968-03-28 | 1969-04-08 | Du Pont | Titanium dioxide pigment coated with silica and alumina |
CN85103475A (en) * | 1985-04-30 | 1986-10-29 | 河南师范大学 | Preparation of rutile type pigment titanium white by high activity crystal |
CN86101534A (en) * | 1986-08-07 | 1988-02-17 | 上海京华化工厂 | The preparation method of water dispersing lide powder pigment |
CN1120978A (en) * | 1994-10-20 | 1996-04-24 | 中国科学院山西煤炭化学研究所 | Method of preparing coated superfine powder with metal surfactant by phase transfer |
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