CN105086522A - Compactly-coated titanium dioxide and compact coating method - Google Patents
Compactly-coated titanium dioxide and compact coating method Download PDFInfo
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- CN105086522A CN105086522A CN201510518688.7A CN201510518688A CN105086522A CN 105086522 A CN105086522 A CN 105086522A CN 201510518688 A CN201510518688 A CN 201510518688A CN 105086522 A CN105086522 A CN 105086522A
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- titanium dioxide
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- tetraethoxy
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Abstract
The invention discloses a compactly-coated titanium dioxide and a compact coating method. The method includes the following steps: mixing titanium dioxide with solvent and pulping the mixture to obtain titanium dioxide pulp; heating the titanium dioxide pulp to the temperature of 40-90 DEG C, adding tetraethoxysilane and inorganic base into the titanium dioxide pulp, and curing the titanium dioxide pulp for 0.5-3 hours to obtain the titanium dioxide pulp coated with silicon dioxide; adjusting the temperature of the titanium dioxide pulp coated with the silicon dioxide to 40-90 DEG C, adding sodium metaaluminate and inorganic acid into the titanium dioxide pulp, continuing curing for 0.5-2 hours, and subjecting the titanium dioxide pulp to filtering, washing, drying and jet milling to obtain the compactly-coated titanium dioxide.
Description
Technical field
The present invention relates to a kind of fine and close coating method of titanium dioxide, and the titanium dioxide of the fine and close coating adopting the method to prepare.
Background technology
Titanium dioxide, due to its semiconductor property, has stronger photocatalytic activity, and the organism contacted with it of degrading under sunlight especially uviolizing, causes the phenomenons such as coating xanthochromia, efflorescence.In order to improve the weathering resistance of TiO 2 pigment, suitable surface treatment is very necessary.General method carries out the process of surface inorganic coating to titanium dioxide, isolated by the organism of titanium dioxide and surrounding, to improve its weathering resistance.Coating substance mainly comprises silicon oxide, aluminum oxide, zirconium white etc.Titanium dioxide weathering resistance after wherein coated with fine and close silicon oxide is best.At present, be silicate or silicon tetrachloride with the silicon raw material of the silicon oxide coated process selection of bibliographical information in production.US Patent No. 2885366, US3928057, US4125412, US5041162, US7682441B2 all uses silicate for raw material, by wet processing coated silica.US Patent No. 6852306B2, US7029648B2 use silicon tetrachloride for raw material is by vapor phase process bag silicon.Publication number CN1850915A and CN1850914A also uses silicate for the coated TiO 2 pigment of raw material.
Summary of the invention
The object of this invention is to provide a kind of fine and close coating method of titanium dioxide, the method take tetraethoxy as raw material cladding titanium dioxide.
Another object of the present invention is to provide a kind of titanium dioxide of fine and close coating.
In order to reach above-mentioned technique effect, the present invention takes following technical scheme:
The invention provides a kind of fine and close coating method of titanium dioxide, comprise the following steps:
Steps A: obtained titania slurry after titanium dioxide and solvent are pulled an oar;
Step B: titania slurry is heated to temperature 40 ~ 90 DEG C, then adds tetraethoxy and mineral alkali in titania slurry, then slaking 0.5 ~ 3h, obtain the titania slurry of coated with silica;
Step C: the temperature of titania slurry regulating coated with silica is 40 ~ 90 DEG C, then adds sodium metaaluminate and mineral acid, then slaking 0.5 ~ 2h, then the titanium dioxide carrying out filtering, wash, obtain after drying fine and close coating.
According to a particular embodiment of the invention, described titanium dioxide is rutile-type or the anatase titanium dioxide of sulfuric acid process or chlorination process production.
According to a particular embodiment of the invention, described titanium dioxide and ethanol or aqueous ethanolic solution or water mix pulls an oar; The concentration of described titania slurry is 100 ~ 500g/L.
According to a particular embodiment of the invention, the add-on of described tetraethoxy is 1% ~ 6% of titanium dioxide quality, and wherein the add-on of tetraethoxy is with SiO
2meter.
According to a particular embodiment of the invention, the add-on of described sodium metaaluminate is 1% ~ 5% of titanium dioxide quality, and the add-on of wherein said sodium metaaluminate is with Al
2o
3meter.
According to a particular embodiment of the invention, described mineral alkali is one or both in ammoniacal liquor, sodium hydroxide; Described mineral acid is one or more in sulfuric acid, hydrochloric acid, nitric acid.
According to a particular embodiment of the invention, described tetraethoxy and mineral alkali adopt downstream feeding mode or cocurrent adding material mode to add in titania slurry; Described downstream feeding mode for be added in titania slurry by tetraethoxy or mineral alkali, more progressively adds mineral alkali or tetraethoxy reacts; Described cocurrent adding material mode is for progressively joining tetraethoxy and mineral alkali in titania slurry simultaneously.
Present invention also offers a kind of titanium dioxide of the fine and close coating obtained by the fine and close coating method preparation of described titanium dioxide.
According to a particular embodiment of the invention, the titanium dioxide of described fine and close coating is at titanium dioxide granule surface the first layer coated silica coating film and second layer coated aluminum oxide coating film.
The present invention is described in detail below.
The invention provides a kind of fine and close coating method of titanium dioxide, comprise the following steps:
Steps A: obtained titania slurry after titanium dioxide and solvent are pulled an oar;
Step B: titania slurry is heated to temperature 40 ~ 90 DEG C, then adds tetraethoxy and mineral alkali in titania slurry, then slaking 0.5 ~ 3h, obtain the titania slurry of coated with silica;
Step C: the temperature of titania slurry regulating coated with silica is 40 ~ 90 DEG C, then adds sodium metaaluminate and mineral acid, then slaking 0.5 ~ 2h, then the titanium dioxide carrying out filtering, wash, obtain after drying fine and close coating.
In the present invention, titania slurry and tetraethoxy react under the katalysis of mineral alkali.Tetraethoxy is hydrolyzed and generates orthosilicic acid under mineral alkali catalysis, and orthosilicic acid is polymerized at titanium dioxide surface, forms silica coating.In the present reaction, mineral alkali is as catalyzer; Titania slurry being heated to temperature 40 ~ 90 DEG C is to reduce energy consumption while of improving rete density; According to a preferred embodiment of the invention, described titania slurry is heated to temperature 50 ~ 80 DEG C.
According to a preferred embodiment of the invention, the temperature regulating the titania slurry of coated with silica is 40 ~ 60 DEG C.
In the present invention, the object of slaking improves silicon or al deposition rate and rete density.Charge temperature and curing temperature too low, rete density decline, temperature is too high, density improve less; Therefore consider density and energy consumption, charge temperature of the present invention and curing temperature are 40 ~ 90 DEG C simultaneously.According to a preferred embodiment of the invention, described curing temperature is 50 ~ 80 DEG C.According to a particular embodiment of the invention, described titanium dioxide is rutile-type or the anatase titanium dioxide of sulfuric acid process or chlorination process production.In the present invention, the particle diameter of titanium dioxide is 200-400nm.
According to a particular embodiment of the invention, described titanium dioxide and ethanol or aqueous ethanolic solution or water mix pulls an oar; The concentration of described titania slurry is 100 ~ 500g/L.In the present invention, mixing ethanol and water volume ratio in the aqueous ethanolic solution of pulling an oar with titanium dioxide is 1:4 ~ 4:1.According to a preferred embodiment of the invention, the concentration of described titania slurry is 150 ~ 350g/L.
According to a particular embodiment of the invention, the add-on of described tetraethoxy is 1% ~ 6% of titanium dioxide quality, and wherein the add-on of tetraethoxy is with SiO
2meter.According to a preferred embodiment of the invention, the add-on of described tetraethoxy is 2% ~ 5% of titanium dioxide quality.
According to a particular embodiment of the invention, the add-on of described sodium metaaluminate is 1% ~ 5% of titanium dioxide quality, and the add-on of wherein said sodium metaaluminate is with Al
2o
3meter.According to a preferred embodiment of the invention, the add-on of described sodium metaaluminate is 3% ~ 4% of titanium dioxide quality.
According to a particular embodiment of the invention, described mineral alkali is one or both in ammoniacal liquor, sodium hydroxide; Described mineral acid is one or more in sulfuric acid, hydrochloric acid, nitric acid.Preferentially select hydrochloric acid during process chloride process titanium dioxide pigment, during process sulfate process titanium dioxide pigment, preferentially select sulfuric acid.
According to a particular embodiment of the invention, described tetraethoxy and mineral alkali adopt downstream feeding mode or cocurrent adding material mode to add in titania slurry; Described downstream feeding mode for be added in titania slurry by tetraethoxy or mineral alkali, more progressively adds mineral alkali or tetraethoxy reacts; Described cocurrent adding material mode is for progressively joining tetraethoxy and mineral alkali in titania slurry simultaneously.
Present invention also offers a kind of titanium dioxide of the fine and close coating obtained by the fine and close coating method preparation of described titanium dioxide.
According to a particular embodiment of the invention, the titanium dioxide of described fine and close coating is at titanium dioxide granule surface the first layer coated silica coating film and second layer coated aluminum oxide coating film.
The present invention compared with prior art, has following beneficial effect:
Present method adopts tetraethoxy as silicon source, and reaction conditions is gentle, and the first titanium dioxide layer after coating is coated with silica film, and the second layer is alumina-coated film, and rete density is high.
Embodiment
Below in conjunction with embodiments of the invention, the invention will be further elaborated.
Embodiment 1:
100g sulfuric acid process rutile type is mixed obtained titania slurry after pulling an oar with 400mL ethanol; Titania slurry is heated to temperature 60 C, then the ammoniacal liquor (ammoniacal liquor volume is 4% of titania slurry volume) that volume ratio is 4% is added, in 120min, add the ethanolic soln of tetraethoxy again, the total amount of tetraethoxy is (with SiO
2meter) be 3% of the first quality of titanium white, then slaking 120min under temperature 60 C, obtains the titania slurry of coated with silica; The temperature regulating the titania slurry of coated with silica is 60 DEG C, then and stream adds the sulfuric acid (quality of sulfuric acid is 10% of sulfuric acid process rutile titanium white quality) that the sodium metaaluminate of 100g/L and concentration are 10%, the total amount of sodium metaaluminate is (with Al
2o
3meter) be 2% of sulfuric acid process rutile type quality, then slaking 90min, then carry out filtering, wash, obtain after dry, comminution by gas stream the titanium dioxide of fine and close coating.
The pigment aluminum weight per-cent of preparation consists of: SiO
2: 2.62%, Al
2o
3: 1.71%.
Embodiment 2:
100g sulfuric acid process rutile type is mixed obtained titania slurry after pulling an oar with 400mL ethanol; Titania slurry is heated to temperature 60 C, and in 120min and stream adds the ammoniacal liquor (ammoniacal liquor volume is 4% of titania slurry volume) that the ethanolic soln of tetraethoxy and volume ratio are 4%, the total amount of tetraethoxy is (with SiO
2meter) be 3% of the first quality of titanium white, then slaking 120min under temperature 60 C, obtains the titania slurry of coated with silica; The temperature regulating the titania slurry of coated with silica is 60 DEG C, then and stream adds the sulfuric acid (quality of sulfuric acid is 10% of sulfuric acid process rutile titanium white quality) that the sodium metaaluminate of 100g/L and concentration are 10%, the total amount of sodium metaaluminate is (with Al
2o
3meter) be titanium white just quality 2%, then slaking 90min, then carry out filtering, wash, obtain after dry, comminution by gas stream the titanium dioxide of fine and close coating.
The pigment aluminum weight per-cent of preparation consists of: SiO
2: 2.58%, Al
2o
3: 1.73%.
Embodiment 3:
Pull an oar except rear obtained titania slurry except being mixed with 1000mL ethanol by 100g sulfuric acid process rutile type, other conditions are identical with embodiment 2.
The pigment aluminum weight per-cent of preparation consists of: SiO
2: 2.69%, Al
2o
3: 1.67%.
Embodiment 4:
Pull an oar except rear obtained titania slurry except being mixed with 200mL ethanol by 100g sulfuric acid process rutile type, other conditions are identical with embodiment 2.
The pigment aluminum weight per-cent of preparation consists of: SiO
2: 2.63%, Al
2o
3: 1.75%.
Embodiment 5:
Pull an oar except rear obtained titania slurry except being mixed with 400mL aqueous ethanolic solution (volume ratio of second alcohol and water is 20:80) by 100g sulfuric acid process rutile type, other conditions are identical with embodiment 2.
The pigment aluminum weight per-cent of preparation consists of: SiO
2: 2.70%, Al
2o
3: 1.68%.
Embodiment 6:
Pull an oar except rear obtained titania slurry except being mixed with 400mL water by 100g sulfuric acid process rutile type, other conditions are identical with embodiment 2.
The pigment aluminum weight per-cent of preparation consists of: SiO
2: 2.57%, Al
2o
3: 1.65%.
Comparative example:
Join in 400mL water by 100g sulfuric acid process rutile type, high-speed stirring is pulled an oar, and adjusts pH to be 10, be heated to 90 DEG C with sodium hydroxide, regulates pH to be 10, drips the sodium silicate solution of 100g/L respectively (with SiO under agitation with two peristaltic pumps
2meter) and 10% dilute sulphuric acid, make slurry pH value remain between 9.8-10.2, the total amount dripping silicon be titanium white just quality 3%, 90min in dropwise, after dropping terminates, slaking 120min.Be 7.0 with sulphur acid for adjusting pH, and stream adds the sodium metaaluminate of 100g/L and the sulfuric acid of 10%, the amount adding sodium metaaluminate is 2% of untreated titania weight (with Al
2o
3meter), maintain pH in the process and add in 6.0-8.0,90min, slaking 60min, regulates pH to be 7.0, recurring 30min.Filter, washing, dry, comminution by gas stream.
The pigment aluminum weight per-cent of preparation consists of: SiO
2: 2.63%, Al
2o
3: 1.83%.
Reduced pigment 1: certain external producer sial coated product;
Reduced pigment 2: certain domestic manufacturer's sial coated product.
Sial coated product, reduced pigment 1 and reduced pigment 2 that the titanium dioxide of the fine and close coating produced by the present embodiment 1-6, comparative example are produced characterize the rete density of prepared TiO 2 pigment by acid-soluble ratio, concrete grammar is as follows, and the data of test are in table 1.
Accurately take testing sample 0.2000g (being accurate to 0.001g) and be placed in 100mL small beaker, accurately measuring 10.0mL66% sulfuric acid joins in small beaker, be placed in 175 DEG C of oil baths, open magnetic agitation, after 60min, take out beaker, add rapidly 40-50ml rubble ice and make sample solution quenching, sample solution is transferred in 100mL volumetric flask after cooling, with distilled water diluting to scale, mixing; After filtration, accurately pipette 10.0mL clear filtrate in 100mL volumetric flask, add 2.0mL20% hydrogen peroxide, with distilled water diluting to scale, shake up, at room temperature static 60min.Be that reference surveys its absorbancy at 410nm wavelength place 1cm cuvette with blank solution.By before with the typical curve of the measured in solution of known titanium dioxide concentration, determine the content dissolving titanium dioxide.
The acid-soluble ratio test result of table 1: embodiment 1-6, comparative example and contrast product
| Sample | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Comparative example | Contrast 1 | Contrast 2 |
| Acid-soluble ratio/% | 4.32 | 3.95 | 3.55 | 4.96 | 4.73 | 5.28 | 7.85 | 4.60 | 8.25 |
As seen from the above table, the TiO 2 pigment prepared by the inventive method relative to taking water glass as the comparative example in silicon source and contrasting commercially available titanium dioxide there is lower acid-soluble ratio, show coated rete there is very high density.
Although with reference to explanatory embodiment of the present invention, invention has been described here, above-described embodiment is only the present invention's preferably embodiment, embodiments of the present invention are not restricted to the described embodiments, should be appreciated that, those skilled in the art can design a lot of other amendment and embodiment, these amendments and embodiment will drop within spirit disclosed in the present application and spirit.
Claims (9)
1. a fine and close coating method for titanium dioxide, is characterized in that described method comprises the following steps:
Steps A: obtained titania slurry after titanium dioxide and solvent are pulled an oar;
Step B: titania slurry is heated to temperature 40 ~ 90 DEG C, then adds tetraethoxy and mineral alkali in titania slurry, then slaking 0.5 ~ 3h, obtain the titania slurry of coated with silica;
Step C: the temperature of titania slurry regulating coated with silica is 40 ~ 90 DEG C, then adds sodium metaaluminate and mineral acid, then slaking 0.5 ~ 2h, then the titanium dioxide carrying out filtering, wash, obtain after drying fine and close coating.
2. the fine and close coating method of titanium dioxide according to claim 1, is characterized in that described titanium dioxide is rutile-type or the anatase titanium dioxide of sulfuric acid process or chlorination process production.
3. the fine and close coating method of titanium dioxide according to claim 1, is characterized in that described titanium dioxide and ethanol or aqueous ethanolic solution or water mix and pulls an oar; The concentration of described titania slurry is 100 ~ 500g/L.
4. the fine and close coating method of titanium dioxide according to claim 1, it is characterized in that the add-on of described tetraethoxy is 1% ~ 6% of titanium dioxide quality, wherein the add-on of tetraethoxy is with SiO
2meter.
5. the fine and close coating method of titanium dioxide according to claim 1, it is characterized in that the add-on of described sodium metaaluminate is 1% ~ 5% of titanium dioxide quality, the add-on of wherein said sodium metaaluminate is with Al
2o
3meter.
6. the fine and close coating method of titanium dioxide according to claim 1, is characterized in that described mineral alkali is one or both in ammoniacal liquor, sodium hydroxide; Described mineral acid is one or more in sulfuric acid, hydrochloric acid, nitric acid.
7. the fine and close coating method of titanium dioxide according to claim 1, is characterized in that described tetraethoxy and mineral alkali adopt downstream feeding mode or cocurrent adding material mode to add in titania slurry; Described downstream feeding mode for be added in titania slurry by tetraethoxy or mineral alkali, more progressively adds mineral alkali or tetraethoxy reacts; Described cocurrent adding material mode is for progressively joining tetraethoxy and mineral alkali in titania slurry simultaneously.
8. the titanium dioxide of the fine and close coating obtained by the fine and close coating method preparation of the titanium dioxide described in any one of claim 1-7.
9. the titanium dioxide of fine and close coating according to claim 8, is characterized in that the titanium dioxide of described fine and close coating is at titanium dioxide granule surface the first layer coated silica coating film and second layer coated aluminum oxide coating film.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107652714A (en) * | 2017-10-31 | 2018-02-02 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method of titanium dioxide densification sial coating |
| CN107722677A (en) * | 2017-11-21 | 2018-02-23 | 攀钢集团攀枝花钢铁研究院有限公司 | Titanium dioxide sial coating method |
| CN108002433A (en) * | 2017-11-30 | 2018-05-08 | 宁波激智科技股份有限公司 | A kind of modified titanium and preparation method thereof and a kind of diffusion barrier |
| CN108061718A (en) * | 2017-12-28 | 2018-05-22 | 安徽中创电子信息材料有限公司 | A kind of fast appraisement method of rutile type titanium white weatherability |
| CN111057271A (en) * | 2019-11-26 | 2020-04-24 | 广东盈骅新材料科技有限公司 | Titanium suboxide composite material and application thereof |
| CN111253781A (en) * | 2020-03-13 | 2020-06-09 | 广东工业大学 | Composite modified titanium dioxide and preparation method and application thereof |
| CN111621171A (en) * | 2020-05-22 | 2020-09-04 | 中信钛业股份有限公司 | Method for improving compactness of silicon dioxide coating layer on surface of titanium dioxide |
| CN113122021A (en) * | 2021-04-16 | 2021-07-16 | 江苏镇钛化工有限公司 | Preparation process for improving weather resistance of titanium dioxide |
| CN111234567B (en) * | 2020-03-18 | 2021-11-05 | 中南大学 | Inorganic coating process for preparing high-weather-resistance titanium dioxide |
| CN114634721A (en) * | 2022-03-01 | 2022-06-17 | 华南理工大学 | Silicon-aluminum oxide coated titanium dioxide and preparation method and application thereof |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107652714A (en) * | 2017-10-31 | 2018-02-02 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method of titanium dioxide densification sial coating |
| CN107722677A (en) * | 2017-11-21 | 2018-02-23 | 攀钢集团攀枝花钢铁研究院有限公司 | Titanium dioxide sial coating method |
| CN108002433A (en) * | 2017-11-30 | 2018-05-08 | 宁波激智科技股份有限公司 | A kind of modified titanium and preparation method thereof and a kind of diffusion barrier |
| CN108061718A (en) * | 2017-12-28 | 2018-05-22 | 安徽中创电子信息材料有限公司 | A kind of fast appraisement method of rutile type titanium white weatherability |
| CN111057271B (en) * | 2019-11-26 | 2021-09-28 | 广东盈骅新材料科技有限公司 | Titanium suboxide composite material and application thereof |
| CN111057271A (en) * | 2019-11-26 | 2020-04-24 | 广东盈骅新材料科技有限公司 | Titanium suboxide composite material and application thereof |
| CN111253781A (en) * | 2020-03-13 | 2020-06-09 | 广东工业大学 | Composite modified titanium dioxide and preparation method and application thereof |
| CN111234567B (en) * | 2020-03-18 | 2021-11-05 | 中南大学 | Inorganic coating process for preparing high-weather-resistance titanium dioxide |
| CN111621171A (en) * | 2020-05-22 | 2020-09-04 | 中信钛业股份有限公司 | Method for improving compactness of silicon dioxide coating layer on surface of titanium dioxide |
| CN111621171B (en) * | 2020-05-22 | 2022-02-08 | 中信钛业股份有限公司 | Method for improving compactness of silicon dioxide coating layer on surface of titanium dioxide |
| CN113122021A (en) * | 2021-04-16 | 2021-07-16 | 江苏镇钛化工有限公司 | Preparation process for improving weather resistance of titanium dioxide |
| CN114634721A (en) * | 2022-03-01 | 2022-06-17 | 华南理工大学 | Silicon-aluminum oxide coated titanium dioxide and preparation method and application thereof |
| CN117476795A (en) * | 2023-12-22 | 2024-01-30 | 宁波长阳科技股份有限公司 | Gap film for photovoltaic module and preparation method thereof |
| CN117476795B (en) * | 2023-12-22 | 2024-04-02 | 宁波长阳科技股份有限公司 | Gap film for photovoltaic module and preparation method thereof |
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Application publication date: 20151125 |