CN100392024C - Titanium dioxide pigment and its preparing method - Google Patents
Titanium dioxide pigment and its preparing method Download PDFInfo
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- CN100392024C CN100392024C CNB2005101229288A CN200510122928A CN100392024C CN 100392024 C CN100392024 C CN 100392024C CN B2005101229288 A CNB2005101229288 A CN B2005101229288A CN 200510122928 A CN200510122928 A CN 200510122928A CN 100392024 C CN100392024 C CN 100392024C
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Abstract
The present invention relates to titanium dioxide pigment and a preparing method thereof and belongs to titanium dioxide pigment with improved durability and optical properties and a producing method thereof. The titanium dioxide pigment of the present invention comprises rutile type or anatase type titanium dioxide particles which are provided with a zirconia coating, an amorphous silica coating and a hydrated alumina coating which are deposited on the particles. The rutile type or anatase type titanium dioxide particle also has an organic coating which is absorbed or bonded on the particles.
Description
Technical field
The present invention relates generally to TiO 2 pigment, and more detailed saying so contained the TiO 2 pigment of Zirconium oxide, Si oxide and aluminum oxide, and this pigment has improved weather resistance and optical property.
Background technology
Titanium dioxide is as a kind of opaque pigment, is widely used in coatings industry, paper plant and as the matting agent of fiber.In order to improve the application performance of TiO 2 pigment, generally all passed through the processing of mineral compound, to improve it such as performances such as weather resistance, whiteness, reducing power and opacifying powers.The TiO 2 pigment that is used for plastics and outdoor coating is except that should having excellent pigment performance, ideal performance is to have weather resistance, that is prevention xanthochromia and atomizing ability, in order to improve weathering resistance, TiO 2 pigment usually carries out coating with one or more hydrous oxides to be handled, and the oxide compound that particularly uses Si is to improve the weathering resistance rank.Using metal hydrate such as silicon and aluminium to be applied to the method that preparation weathering resistance in the titanium dioxide has a TiO 2 pigment of the physics of different levels and optical property has a lot, and as a whole, these processes are in order to produce the TiO of high-weatherability
2, need long treatment time and higher temperature.The present invention adopts Zirconium oxide, Si oxide, aluminum oxide to coat in proper order titanium dioxide is handled, and to obtain needed weather resistance and optical characteristics, this kind mode seemingly keeps performance and cost-efficient a kind of new way.
Disclose an easily preparation technology of the TiO 2 pigment of dispersion, high-durability as Chinese patent CN1578813A, this technology is handled based on Si, Al, and carries out under higher temperature, does not consider the oxide compound of deposition one deck zirconium before the Si deposition.
U.S. Pat 5730796 proposes a kind of method for preparing durable pigments, this pigment has the amorphous silicon oxide coating of cerium oxide layer coating, one deck densification, with preferred one deck aluminum oxide coating layer, do not mention or advise the purposes of the oxide compound of deposition one deck zirconium before the Si deposition to raising pigment weather resistance and optical property.
Chinese patent CN1244888A discloses a kind of TiO 2 pigment that contains titanium dioxide core, described titanium dioxide core by the coprecipitate of the oxyhydroxide of the oxyhydroxide of the oxyhydroxide of the oxyhydroxide of one deck zirconium or zirconium, one deck titanium or titanium, one deck phosphoric acid salt and silicon-dioxide, then layer of aluminum oxyhydroxide order coat, do not mention that the order of Zirconium oxide, Si oxide and aluminum oxide coats.
The order that above-mentioned these patents are not all mentioned Zirconium oxide, Si oxide and aluminum oxide is coated on the application in the wet processing of surface of pigments deposition.
Summary of the invention
An object of the present invention is to provide a kind of TiO 2 pigment that has favorable durability and optical characteristics in industrial application such as plastics and coating, the order that described TiO 2 pigment has passed through Zirconium oxide, Si oxide, aluminum oxide coats.Another object of the present invention is the method for producing above-mentioned TiO 2 pigment.
According to design provided by the present invention, this TiO 2 pigment comprise by one deck Zirconium oxide, one deck Si oxide, layer of aluminum oxide compound the order rutile-type or the anatase titanium dioxide particle that coat;
The content of above-mentioned Zirconium oxide is 0.2～1% of titanium dioxide granule, and the content of Si oxide is 1～2% of titanium dioxide granule, and the content of aluminum oxide is 3～5% of titanium dioxide granule, and unit is a weight percentage.
A kind of production method of TiO 2 pigment comprises:
(1), forms the aqeous suspension of TiO 2 pigment;
(2), under the condition that has dispersion agent to exist, grind the aqeous suspension of the TiO 2 pigment that forms in (1);
(3), the aqeous suspension with the TiO 2 pigment after the milled processed in (2) is diluted to 250～350g/l;
(4), will be heated to 50～80 ℃ through the aqeous suspension after (3) processing;
(5), add the enough zirconium compounds aqueous solution in the aqeous suspension after handling, account for the zirconium dioxide layer of titanium dioxide granule weight 0.1～1.5% in the suspension at particle surface deposition one deck through (4);
(6), add in the alkali lye and slip in the aqeous suspension in 0.5～1.5 hour after handling, form the TiO 2 pigment aqeous suspension that the surface is coating one deck zirconium dioxide through (5);
(7), will be adjusted to 8～11 through the pH value of the aqeous suspension after (6) processing with alkali lye;
(8), in 1～2 hour, in suspension, add enough aqueous silicate solutions, keep pH value 8～11 with mineral acid simultaneously, deposit the silicon dioxide layer that one deck accounts for titanium dioxide granule weight 1～3% in the suspension at particle surface;
(9), the sodium aluminate aqueous solution that adds q.s in the aqeous suspension after handling through (8), reach 7～9 by the pH value that adds alum liquor adjusting formation suspension, make on the surface that is coating zirconium dioxide and silicon-dioxide, deposition one deck alumina layer, alumina weight account for 3～5% of titanium dioxide granule weight in the suspension;
(10), the aqeous suspension pH value of regulating after handling through (9) is 6.5～7.5, then with the mixture slaking of formation 1～2 hour.
Utilize again known method to the TiO 2 pigment aqeous suspension filter, wash, dry, micronizing and organic process.
The concentration of the aqeous suspension of the TiO 2 pigment that forms is 500～700g/l.Reasonable concentration is 550～650g/l.Described dispersion agent is phosphoric acid salt or silicate.Phosphoric acid salt wherein is Sodium hexametaphosphate 99, and silicate is water glass.The Heating temperature of described aqeous suspension is 60 ℃.
Described zirconium compounds is a kind of in zirconium sulfate or zirconium chloride or basic zirconium chloride or all the other the hydrolyzable zirconium compoundss or their mixture.The alkali lye that uses is NaOH.Add sodium aluminate solution and Tai-Ace S 150 simultaneously and regulate the pH value of aqeous suspension.
A kind of improved method for preparing titanium dioxide pigment particles, wherein the particle in the titanium dioxide hydrous slurry is carried out wet processing with the aqueous solution of zirconium compounds, silicate and aluminum compound, the TiO 2 pigment that obtains has the zirconium white of the first layer and silicon oxide and three coating layers of trilaminar aluminum oxide of the second layer, improvement wherein is included in before the compound deposition of silicon, the compound of deposition one deck zirconium.
Embodiment
Of the present invention have the TiO 2 pigment that improves weather resistance and optical property and comprise by the rutile-type or the anatase titanium dioxide particle of the order coating of the oxide compound of the oxide compound of the oxide compound of one deck zirconium, one deck silicon, layer of aluminum institute.
The method for preparing above-mentioned TiO 2 pigment comprises each step in the following order:
(1). form the aqeous suspension of TiO 2 pigment,
(2). under the condition that has dispersion agent to exist, grind the aqeous suspension of the TiO 2 pigment that forms in (1),
(3). the aqeous suspension of the TiO 2 pigment after the milled processed in (2) is diluted to 250g/l～350g/l,
(4). the aqeous suspension of the TiO 2 pigment after the dilution process in (3) is heated to 50～80 ℃,
(5). in aqeous suspension, add the enough zirconium compounds aqueous solution, deposit the zirconium dioxide layer that one deck accounts for titanium dioxide granule weight 0.1% to 1.5% in the suspension at particle surface,
(6). in 0.5 to 1.5 hour, add in the alkali lye and slip, form the TiO 2 pigment aqeous suspension that the surface is coating one deck zirconium dioxide,
(7) with alkali lye the pH value of suspension is adjusted to 8～11,
(8). in 1 hour to 2 hours, in suspension, add enough aqueous silicate solutions, keep the pH value 8～11 with mineral acid simultaneously, deposit the silicon dioxide layer that one deck accounts for titanium dioxide granule weight 1% to 3% in the suspension at particle surface,
(9). in suspension, add the sodium aluminate aqueous solution of q.s, regulate pH value to 7～9 that form suspension by adding alum liquor, make on the surface that is coating zirconium dioxide and silicon-dioxide, deposition one deck alumina layer, alumina weight accounts for 3% to 5% of titanium dioxide granule weight in the suspension
(10). regulating the pH of suspension value is 6.5～7.5, then with the mixture slaking that forms 1 to 2 hour.
(11). utilize known method to the TiO 2 pigment aqeous suspension filter, wash, dry, micronizing and organic process.
The inventive method may be carried out batchwise also and can carry out continuously.
Of the present invention improving one's methods can be used to handle anatase titanium dioxide or the rutile titanium dioxide pigment that makes in any form, anatase titanium dioxide pigment of for example having known that is made by sulfuric acid process and the rutile titanium dioxide pigment that is made by sulfuric acid process or chlorination process technology.
The first step of the inventive method comprises the aqeous suspension that forms processed TiO 2 pigment, suspension concentration is 500～700g/l, preferably about 600g/l, advantageously, after the aqeous suspension that forms TiO 2 pigment, regulating suspension is the alkaline pH value, and advantageously, the pH value of regulating suspension is 9.5～10.5.
Second step of the inventive method comprises grinds the aqeous suspension that forms in the first step, can adopt known wet-milling mode to carry out, as ball milling, sand milling etc., preferably select the mode of sand milling for use, best is the aqeous suspension that forms in the first step to be disperseed to stir for some time in advance before sand milling, as 30 minutes, preferred dispersing agent is a phosphoric acid salt, Sodium hexametaphosphate 99 more preferably, the preferred dispersing agent consumption is 0.05% to 1%, weight with described paint material is benchmark, and more the preferred dispersing agent consumption is 0.1% to 0.5%, and highly preferred dispersant dosage is 0.3%.
It is preferred to 350g/l that aqeous suspension in the step (3) is diluted to 300g/l, and best is to be diluted to 320～330g/l.
In the methods of the invention, the zirconium compounds aqueous solution that adds in the step (5) should be enough to provide described first coating, is benchmark with the weight of described paint material, and its amount is for about 0.1% to 1.5%, and preferably 0.5% to 1%, preferred zirconium compounds is a zirconium sulfate.
In the methods of the invention, the aqueous silicate solution in the step (8) should be enough to provide described second coating, and preferred silicate is water glass, weight with described paint material is benchmark, its amount is for about 1% to 3%, and preferably 1.5% to 4%, best is 1.7%.Mineral acid can be a kind of in sulfuric acid, nitric acid, hydrochloric acid, the carbonic acid, preferably sulfuric acid.Preferably with sulfuric acid the pH value is maintained 9～10, best is with sulfuric acid the pH value to be maintained about 9.5.
In the methods of the invention, carry out aluminium in the step (9) when coating, sodium aluminate and Tai-Ace S 150 add simultaneously, regulate pH value at 7～9 according to the fluctuations in discharge of Tai-Ace S 150, preferably with Tai-Ace S 150 adjusting pH value 7.5～8.5, more preferably 7.8～8.2.
In the methods of the invention, when each encapsulation steps finishes, be comparatively favourable more than 30 minutes with the suspension slaking, this helps each abundant deposition that coats the section oxide compound.
After finishing described oxide compound coating, TiO 2 pigment is adopted that known method is washed, filtered, carries out organic process during dry, micronizing, strengthen the dispersiveness of described TiO 2 pigment in application system, organic process can adopt the method for wet method to carry out, also can when micronizing, add, organic agent comprises known trimethylolethane, TriMethylolPropane(TMP) and siloxanes etc.
With reference to following embodiment, but be not limited thereto, will understand the present invention better.
Embodiment 1
With deionized water with the undressed TiO of 1500g
2Allotment is into about the aqeous suspension of 600g/l, with NaOH solution the pH value of aqeous suspension is transferred to 9.8, the sodium hexametaphosphate solution of adding 0.3%, grind 30min with sand mill, remove sand, then, suspension is diluted to 4.7L, temperature is raised to 60 ℃, and the form with zirconium sulfate solution in 1 hour adds 9 gram ZrO
2, the NaOH solution with 15% in 1 hour is regulated pH value to 8, slaking 30 minutes, and the form with sodium silicate solution adds 25.5 gram SiO in 1.5 hours then
2, use 30% H simultaneously
2SO
4Keep the pH value about 9.5, slaking 30 minutes, the form with sodium aluminate solution adds 30 gram Al in 2 hours again
2O
3, keep the pH value about 8.0 with alum liquor simultaneously, with suspension slaking 30min, regulating the pH of suspension value is 6.5～7.5, then with the mixture slaking that forms 1～2 hour.With suspension slaking 30 minutes, with sulfuric acid the pH value is adjusted to 7.0, slaking 30 minutes.With gained sample filtering, washing, drying, and carry out micronization.
Embodiment 2
With deionized water with the undressed TiO of 1500g
2Allotment is into about the suspension of 600g/l, with NaOH solution the pH value of suspension is transferred to 9.8, the sodium hexametaphosphate solution of adding 0.3%, grind 30min with sand mill, remove sand, then, suspension is diluted to 4.7L, temperature is raised to 60 ℃, regulates pH of suspension value to 10.0 with NaOH (15%) solution, and the form with sodium silicate solution adds 25.5gSiO in 1.5 hours then
2, use H simultaneously
2SO
4(30%) keep the pH value about 9.5, slaking 30 minutes, the form with sodium aluminate solution adds 30gAl in 2 hours again
2O
3, keep the pH value about 8.0, with suspension slaking 30min (10) with alum liquor simultaneously. and regulating the pH of suspension value is 6.5～7.5, then with the mixture slaking that forms 1 to 2 hour.With suspension slaking 30 minutes, with sulfuric acid the pH value is adjusted to 7.0, slaking 30 minutes.With gained sample filtering, washing, drying, and carry out micronization.
Embodiment 3
Repeat the processing of embodiment 1, pigment is with 0.3% TriMethylolPropane(TMP) micronization.
Reduced pigment
Use has the commercially available pigment of following feature:
Reduced pigment 1: adopt fine and close silicon, heavily the pigment of Bao Fuing
Reduced pigment 2: the pigment that is used for single aluminium coating of coating
Reduced pigment 3: uncoated pigment
The foregoing description and Comparative Examples result summary are in following table
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Contrast 1 | Contrast 2 | Contrast 3 | |
| Whiteness | 101.2 | 99.7 | 101.6 | 97.8 | 100.9 | 100 |
| Reducing power | 1920 | 1880 | 1930 | 1800 | 1930 | 1900 |
| Dispersed | 38 | 41 | 36 | 62 | 40 | 55 |
| Resistance to chalking | 1 | 2 | 1 | 1 | 2 | 3 |
Can see that TiO 2 pigment of the present invention has good weather resistance, splendid optical property according to the foregoing description and last table.
Therefore, the present invention is well suited for realization purpose of the present invention and reaches above-mentioned result and advantage and be institute of the present invention those character of inherent.Although those skilled in the art can make many modifications to the present invention, these modifications are included in the scope of the present invention of claims qualification.
Claims (12)
1. a TiO 2 pigment is characterized in that, it comprise by one deck Zirconium oxide, one deck Si oxide, layer of aluminum oxide compound the order rutile-type or the anatase titanium dioxide particle that coat; Wherein, the content of Zirconium oxide is 0.2～1% of titanium dioxide granule, and the content of Si oxide is 1～2% of titanium dioxide granule, and the content of aluminum oxide is 3～5% of titanium dioxide granule, and unit is a weight percentage.
2. the production method of a TiO 2 pigment comprises:
(1), forms the aqeous suspension of TiO 2 pigment;
(2), under the condition that has dispersion agent to exist, grind the aqeous suspension of the TiO 2 pigment that forms in (1);
(3), the aqeous suspension with the TiO 2 pigment after the milled processed in (2) is diluted to 250～350g/l;
(4), will be heated to 50～80 ℃ through the aqeous suspension after (3) processing;
(5), add the enough zirconium compounds aqueous solution in the aqeous suspension after handling, account for the zirconium dioxide layer of titanium dioxide granule weight 0.1～1.5% in the suspension at particle surface deposition one deck through (4);
(6), add in the alkali lye and slip in the aqeous suspension in 0.5～1.5 hour after handling, form the TiO 2 pigment aqeous suspension that the surface is coating one deck zirconium dioxide through (5);
(7), will be adjusted to 8～11 through the pH value of the aqeous suspension after (6) processing with alkali lye;
(8), in 1～2 hour, add enough aqueous silicate solutions in the suspension after handling through step (7), keep the pH value 8～11 with mineral acid simultaneously, deposit the silicon dioxide layer that one deck accounts for titanium dioxide granule weight 1～3% in the suspension at particle surface;
(9), the sodium aluminate aqueous solution that adds q.s in the aqeous suspension after handling through (8), reach 7～9 by the pH value that adds alum liquor adjusting formation suspension, make on the surface that is coating zirconium dioxide and silicon-dioxide, deposition one deck alumina layer, alumina weight account for 3～5% of titanium dioxide granule weight in the suspension;
(10), the aqeous suspension pH value of regulating after handling through (9) is 6.5～7.5, then with the mixture slaking of formation 1～2 hour.
3. as the production method of TiO 2 pigment as described in the claim 2, its feature also is, utilize again known method to the TiO 2 pigment aqeous suspension of handling the back through step (10) and forming filter, wash, dry, micronizing and organic process.
4. as the production method of TiO 2 pigment as described in the claim 2, it is characterized in that the concentration of the aqeous suspension of the TiO 2 pigment of step (1) is 500～700g/l.
5. as the production method of TiO 2 pigment as described in the claim 4, it is characterized in that the concentration of the aqeous suspension of the TiO 2 pigment in the step (1) is 550～650g/l.
6. as the production method of TiO 2 pigment as described in the claim 2, it is characterized in that dispersion agent is phosphoric acid salt or silicate.
7. as the production method of TiO 2 pigment as described in the claim 6, it is characterized in that phosphoric acid salt is Sodium hexametaphosphate 99, silicate is water glass.
8. as the production method of TiO 2 pigment as described in the claim 2, it is characterized in that the Heating temperature of aqeous suspension is 60 ℃ in the step 4.
9. as the production method of TiO 2 pigment as described in the claim 2, it is characterized in that zirconium compounds is a kind of in zirconium sulfate or zirconium chloride or basic zirconium chloride or all the other the hydrolyzable zirconium compoundss or their mixture.
10. as the production method of TiO 2 pigment as described in the claim 2, it is characterized in that the alkali lye that uses is NaOH.
11. the method as in the claim 2 is characterized in that, adds the pH value that sodium aluminate solution and Tai-Ace S 150 are regulated aqeous suspension simultaneously.
12. improved method for preparing titanium dioxide pigment particles, wherein the particle in the titanium dioxide hydrous slurry is carried out wet processing with the aqueous solution of zirconium compounds, silicate and aluminum compound, the TiO 2 pigment that obtains has the zirconium white of the first layer and silicon oxide and three coating layers of trilaminar aluminum oxide of the second layer, improvement wherein is included in before the compound deposition of silicon, the compound of deposition one deck zirconium.
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| CNB2005101229288A CN100392024C (en) | 2005-12-05 | 2005-12-05 | Titanium dioxide pigment and its preparing method |
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| CN100392024C true CN100392024C (en) | 2008-06-04 |
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| CN109853067A (en) * | 2019-03-01 | 2019-06-07 | 华东理工大学 | A kind of preparation method of viscose rayon delustring titanium dioxide |
| CN110484026B (en) * | 2019-08-26 | 2020-07-14 | 中东金润新材料有限公司 | Production process of chemical fiber grade titanium dioxide |
| CN111073352B (en) * | 2019-12-31 | 2021-10-26 | 南京钛白化工有限责任公司 | Preparation method of low-photoactivity flatting agent for chemical fibers |
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Assignee: SHANDONG DAWN TITANIUM INDUSTRY CO., LTD. Assignor: Wuxi Haopu Titanium Co., Ltd. Contract record no.: 2012370000107 Denomination of invention: Ultrafine rutile type titanium dioxide pigment special for color master and preparation method thereof Granted publication date: 20080604 License type: Exclusive License Open date: 20060524 Record date: 20120425 |
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Effective date of registration: 20191008 Address after: 243000 Anhui city of Ma'anshan province at Xinhua Economic Development Zone, Road No. 1 Patentee after: Anhui Venus Titanium White (Group) Co., Ltd. Address before: 214194 Beizhen Jing Zhang Jing Industrial Zone, Xishan District, Jiangsu, Wuxi Patentee before: Wuxi Haopu Titanium Co., Ltd. |
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