CN109321002A - A kind of preparation method of chloride process titanium dioxide silicon zirconium aluminium ternary coating - Google Patents
A kind of preparation method of chloride process titanium dioxide silicon zirconium aluminium ternary coating Download PDFInfo
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The present invention relates to a kind of preparation methods of chloride process titanium dioxide silicon zirconium aluminium ternary coating, step are as follows: titanium dioxide is configured to the suspension that concentration is 500~600g/L with distilled water by A., adjusting pH value with NaOH aqueous solution is 9.5~10.5, and sodium metasilicate is added and stirs obtained titania slurry；B. 60~80min of grinding distribution is carried out to slurry with sand mill；C. slurry after grinding distribution is squeezed into coating tank and is warming up to 60~80 DEG C；D. zirconium sulfate aqueous solution and aluminum sulfate aqueous solution, constant temperature stirring is added with cocurrent；Adjusting pH value with NaOH is 7.0~8.0, and insulated and stirred cures 90~120min；E. washing is filtered to the silicon zirconium aluminium coating titanium dioxide after curing with 50~60 DEG C of distilled water；F. expansion drying and air-flow crushing are carried out to the silicon zirconium aluminium ternary coating titanium dioxide after filtration washing, the titanium dioxide of silicon zirconium aluminium ternary coating is made.Present invention process process is simple, easy to operate, energy conservation and environmental protection, and titanium dioxide has good glossiness, water dispersible and weatherability after ternary coating.
Description
Technical field
The invention belongs to chemical production technical fields, and in particular to a kind of chloride process titanium dioxide silicon zirconium aluminium ternary coating
Preparation method.
Background technique
Titanium dioxide has superior whiteness, reducing power, weatherability, heat resistance and chemical stability, especially non-toxic,
It can be widely applied to the fields such as coating, plastics, papermaking, ink, chemical fibre, rubber, cosmetics, food and medicine.Titanium dioxide
Main production is sulfuric acid process and chloridising, and sulfuric acid process is traditional handicraft, and this method is complicated for operation, long flow path, environment are dirty
Dye is big, and chloridising production technology is advanced, and production capacity is big, and comprehensive energy consumption is low, good product quality, and chlorine is Ke Xunhuanliyong, mistake
Journey is simple, it can be achieved that intelligent operation, is greatly reduced human resources, becomes at present the master of titanium dioxide production technique in the world
Stream trend.
Due to titanium dioxide photochemical activity with higher, photochemical reaction can occur under illumination condition, can break
Bad organic substance seriously affects product phenomena such as causing material weatherability decrease, easy dusting, xanthochromia, be cracked, fall off
Service life and performance.Simultaneously because titanium dioxide is a kind of substance of hydrophilic and oleophobic, the titanium dioxide that surface does not coat is each
Dispersibility in kind solvent and water paint is poor.Titanium dioxide preparation process can not change its photochemistry defect, can only reduce
Its photochemical activity assigns titanium dioxide for performances such as the dispersibility, optical stability and the weatherabilities that improve titanium dioxide
Application performance, it is necessary to its surface carry out coating processing.
The most inorganic coating of domestic and international application is the oxide of the substances such as silicon, aluminium, zirconium, cerium and manganese, i.e., in a certain concentration
Titanium dioxide slurries in, acid or alkaline coating agent is added, then neutralize with alkali or acid, makes coating agent under certain condition with water
Close oxide form be deposited in particle surface, but use single oxide as film forming matter there are many deficiencies, no
The requirement that weatherability and dispersibility improve can be reached, thus often carry out binary or multiple elements design coating.Due to composite coated
Complex technical process, realization is relatively difficult, therefore domestic and international researcher is fewer.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of chloride process titanium dioxide silicon zirconium aluminium ternary coating, to chlorination
The rutile titanium dioxide of method production carries out silicon zirconium aluminium ternary coating, optimizes coating process process, improves coating titanium dioxide
Glossiness, water dispersible and high-weatherability.
The technical solution adopted by the present invention is that: the preparation method of chloride process titanium dioxide silicon zirconium aluminium ternary coating, including with
Lower step:
A, titanium dioxide prepared by chloridising slurry preparation: is configured to concentration as the two of 500~600g/L with distilled water
Titanium oxide suspension is 9.5~10.5 with the pH value that NaOH aqueous solution adjusts tio_2 suspension, adds the inclined silicon of dispersing agent
Then sour sodium stirs 20~30min with the revolving speed of 300~400r/min, titania slurry is made；
B, slurry is ground: the prepared titania slurry of step A is carried out 60~80min of grinding distribution with sand mill；
C, slurry heats up: titania slurry after grinding distribution being squeezed into coating tank, is warming up to 60~80 DEG C；
D, silicon zirconium aluminium coating: with two peristaltic pumps, zirconium sulfate aqueous solution and aluminum sulfate aqueous solution, sulfuric acid is added in cocurrent simultaneously
The additional amount of aqueous zirconium is with ZrO2It is calculated as TiO in slurry2The 2.0~3.0% of quality, the additional amount of aluminum sulfate aqueous solution with
Al2O3It is calculated as TiO in slurry2The 2.5~3.5% of quality, adition process is maintained at 60~80 DEG C of temperature, with 600~800r/min
Revolving speed stirring；Adjusting slurry pH value with NaOH aqueous solution after adding is 7.0~8.0, continuation insulated and stirred curing 90~
120min generates silicon zirconium aluminium coating titanium dioxide；
E, washing filtration washing: is filtered extremely to the silicon zirconium aluminium coating titanium dioxide after curing with 50~60 DEG C of distilled water
Filtrate conductivity is less than 10 μ s/cm；
F, expansion drying and air-flow powder drying, crushing: are carried out to the silicon zirconium aluminium ternary coating titanium dioxide after filtration washing
It is broken, the titanium dioxide of silicon zirconium aluminium ternary coating is made.
The additional amount of sodium metasilicate is with SiO2It is calculated as TiO in slurry2The 2.0~3.0% of quality, zirconium sulfate aqueous solution concentration
With ZrO2It is calculated as 80~100g/L, aluminum sulfate aqueous solution concentration is with Al2O3It is calculated as 90~110g/L, sodium hydrate aqueous solution concentration
For 100~200g/L.With the addition time of peristaltic pump cocurrent addition simultaneously zirconium sulfate aqueous solution and aluminum sulfate aqueous solution in step D
For 40~60min.After step B grinding in titania slurry titanium dioxide average grain diameter≤1.0 μm.It is obtained in step F
Average grain diameter≤0.30 μm of silicon zirconium aluminium ternary coating titanium dioxide.Titanium dioxide is the rutile-type titanium dioxide of chloridising preparation
Titanium.
The technical indicator of the rutile titanium dioxide of chloridising preparation are as follows: TiO2Content >=92wt%, average grain diameter≤
5.0 μm, rutile TiO2Content >=97wt%, pH value 6.5~8.5, sieve residue (45 μm)≤0.06%, value >=97 L, moisture
Dissipate property >=49%, reducing power (Reynolds number) >=1300.
Compared with prior art, the beneficial effects of the present invention are: 1. to chloridising production rutile titanium dioxide into
The processing of row silicon zirconium aluminium ternary envelope membrane surface, reduces the catalytic activity of titanium dioxide, improves its water dispersible, improve simultaneously
The performances such as its weatherability and anti-powdering.2. slurry pH value is adjusted with NaOH, dispersing agent sodium metasilicate is added in slurry preparation,
Optimize titanium dioxide dispersion effect in water, no precipitating formation, it is ensured that the uniformity of coating.In addition sodium metasilicate, also conduct
Grinding aid and SiO2Coating agent, it is molten when cocurrent is gradually added into zirconium sulfate and aluminum sulfate solution under the conditions of 60~80 DEG C
The pH value of liquid is gradually reduced, and sodium metasilicate starts to hydrolyze to form SiO2Cladding is deposited on titanium dioxide surface.3. in the slurry
Zirconium sulfate and aluminum sulfate mixture solution is added simultaneously in cocurrent, under the conditions of 60~80 DEG C, adjusts slurry pH value with NaOH aqueous solution
It is 7.0~8.0, zirconium oxide and aluminium oxide co-precipitation are chemically reacted while being carried out, and are then cured again, in titanium dioxide surface
Form silicon zirconium aluminium ternary coating.4. coating with short production cycle, advantageously reduces energy consumption, save production cost.
Zirconium sulfate water is added using cocurrent simultaneously in the preparation method of chloride process titanium dioxide silicon zirconium aluminium ternary coating of the present invention
Solution and aluminum sulfate aqueous solution, co-precipitation chemical reaction carry out silicon zirconium aluminium three to the rutile titanium dioxide of chloridising production
First coating, technical process is simple, easy to operate, energy conservation and environmental protection, improves the quality of titanium dioxide, titanium dioxide after ternary coating
With good glossiness, water dispersible and weatherability.
Specific embodiment
The following describes the present invention in detail with reference to examples.The scope of protection of the present invention is not limited to the embodiment, this field
Technical staff makes any change within the scope of the claims and also belongs to the scope of protection of the invention.
Embodiment 1
The preparation method of chloride process titanium dioxide silicon zirconium aluminium ternary coating of the present invention, comprising the following steps:
A, titanium dioxide prepared by chloridising slurry preparation: is configured to the titanium dioxide that concentration is 500g/L with distilled water
The pH value that the NaOH aqueous solution that suspension is 100g/L with concentration adjusts tio_2 suspension is 9.5, and it is inclined to add dispersing agent
Sodium metasilicate, additional amount is with SiO2It is calculated as TiO in slurry2Then the 2.0% of quality stirs 20min, system with the revolving speed of 300r/min
Obtain titania slurry；
B, slurry is ground: by the prepared titania slurry of step A, being carried out grinding distribution 60min with sand mill, is ground
Average grain diameter≤1.0 μm of titanium dioxide afterwards；
C, slurry heats up: titania slurry after step B grinding being squeezed into coating tank, is warming up to 60 DEG C；
D, silicon zirconium aluminium coating: zirconium sulfate aqueous solution is added with peristaltic pump, additional amount is with ZrO2It is calculated as TiO in slurry2Quality
2.0%, the concentration of zirconium sulfate aqueous solution is with ZrO2It is calculated as 80g/L；Aluminum sulfate aqueous solution is added with peristaltic pump cocurrent simultaneously, is added
Amount is with Al2O3It is calculated as TiO in slurry2The 2.5% of quality, the concentration of aluminum sulfate aqueous solution is with Al2O3It is calculated as 90g/L, zirconium sulfate is molten
The time is added as 40min in liquid and aluminum sulfate solution cocurrent, and adition process is maintained at 60 DEG C of temperature, is stirred with the revolving speed of 600r/min
It mixes；It is 7.0 that the NaOH aqueous solution for being 100g/L with concentration after adding, which adjusts slurry pH value, continues insulated and stirred and cures 90min,
Generate silicon zirconium aluminium coating titanium dioxide；
E, filtration washing: the silicon zirconium aluminium coating titanium dioxide after curing in step D is filtered with 50 DEG C of distilled water and is washed
It washs to filtrate conductivity less than 10 μ s/cm；
F, drying, crushing: to after filtration washing in step E silicon zirconium aluminium ternary coating titanium dioxide carry out expansion drying and
The titanium dioxide of silicon zirconium aluminium ternary coating is made in air-flow crushing.
Embodiment 2
The following steps are included:
A, titanium dioxide prepared by chloridising slurry preparation: is configured to the titanium dioxide that concentration is 550g/L with distilled water
The pH value that the NaOH aqueous solution that suspension is 150g/L with concentration adjusts tio_2 suspension is 10.0, adds dispersing agent
Sodium metasilicate, additional amount is with SiO2Meter is TiO in slurry2Then the 2.5% of quality stirs 25min, system with revolving speed 350r/min
Obtain titania slurry；
B, slurry is ground: being carried out grinding distribution 70min to the prepared titania slurry of step A with sand mill, is ground
Average grain diameter≤1.0 μm of titanium dioxide afterwards；
C, slurry heats up: titania slurry after step B grinding being squeezed into coating tank, is warming up to 70 DEG C；
D, silicon zirconium aluminium coating: zirconium sulfate aqueous solution is added with peristaltic pump, additional amount is with ZrO2It is calculated as TiO in slurry2Quality
2.5%, the concentration of zirconium sulfate aqueous solution is with ZrO2It is calculated as 90g/L；Aluminum sulfate aqueous solution is added with peristaltic pump cocurrent simultaneously, is added
Amount is with Al2O3It is calculated as TiO in slurry2The 3.5% of quality, the concentration of aluminum sulfate aqueous solution is with Al2O3It is calculated as 100g/L, zirconium sulfate is molten
The time is added as 40min in liquid and aluminum sulfate solution cocurrent, and adition process is maintained at 70 DEG C of temperature, is stirred with the revolving speed of 700r/min
It mixes；It is 7.5 that the NaOH aqueous solution for being 150g/L with concentration after adding, which adjusts slurry pH value, continues insulated and stirred curing
100min generates silicon zirconium aluminium coating titanium dioxide；
E, filtration washing: the silicon zirconium aluminium coating titanium dioxide after curing in step D is filtered with 55 DEG C of distilled water and is washed
It washs to filtrate conductivity less than 10 μ s/cm；
F, drying, crushing: to after filtration washing in step E silicon zirconium aluminium ternary coating titanium dioxide carry out expansion drying and
The titanium dioxide of silicon zirconium aluminium ternary coating is made in air-flow crushing.
Embodiment 3
The following steps are included:
A, titanium dioxide prepared by chloridising slurry preparation: is configured to the titanium dioxide that concentration is 600g/L with distilled water
The pH value that the NaOH aqueous solution that suspension is 200g/L with concentration adjusts tio_2 suspension is 10.5, adds dispersing agent
Sodium metasilicate, additional amount is with SiO2It is calculated as TiO in slurry2The 3.0% of quality stirs 30min, system then with revolving speed 400r/min
Obtain titania slurry；
B, slurry is ground: being carried out grinding distribution 80min to the prepared titania slurry of step A with sand mill, is ground
Average grain diameter≤1.0 μm of titanium dioxide afterwards；
C, slurry heats up: titania slurry after step B grinding being squeezed into coating tank, is warming up to 80 DEG C；
D, silicon zirconium aluminium coating: zirconium sulfate aqueous solution is added with peristaltic pump, additional amount is with ZrO2It is calculated as TiO in slurry2Quality
3.0%, the concentration of zirconium sulfate aqueous solution is with ZrO2It is calculated as 100g/L；Aluminum sulfate aqueous solution is added with peristaltic pump cocurrent simultaneously, adds
Enter amount with Al2O3It is calculated as TiO in slurry2The 3.5% of quality, the concentration of aluminum sulfate aqueous solution is with Al2O3It is calculated as 110g/L, zirconium sulfate
The time is added as 60min in solution and aluminum sulfate solution cocurrent, and adition process is maintained at 80 DEG C of temperature, is stirred with the revolving speed of 800r/min
It mixes；It is 8.0 that the NaOH aqueous solution for being 200g/L with concentration after adding, which adjusts slurry pH value, continues insulated and stirred curing
110min generates silicon zirconium aluminium coating titanium dioxide；
E, filtration washing: the silicon zirconium aluminium coating titanium dioxide after curing in step D is filtered with 60 DEG C of distilled water and is washed
It washs to filtrate conductivity less than 10 μ s/cm；
F, drying, crushing: to after filtration washing in step E silicon zirconium aluminium ternary coating titanium dioxide carry out expansion drying and
The titanium dioxide of silicon zirconium aluminium ternary coating is made in air-flow crushing.
Embodiment 4
The following steps are included:
A, titanium dioxide prepared by chloridising slurry preparation: is configured to the titanium dioxide that concentration is 550g/L with distilled water
The pH value that the NaOH aqueous solution that suspension is 200g/L with concentration adjusts tio_2 suspension is 10.5, adds dispersing agent
Sodium metasilicate, additional amount is with SiO2It is calculated as TiO in slurry2The 2.5% of quality stirs 25min, system then with revolving speed 400r/min
Obtain titania slurry；
B, slurry is ground: with sand mill to the prepared titania slurry of step A, carrying out grinding distribution 70min, grinding
Average grain diameter≤1.0 μm of titanium dioxide afterwards；
C, slurry heats up: titania slurry after step B grinding being squeezed into coating tank, is warming up to 75 DEG C；
D, silicon zirconium aluminium coating: zirconium sulfate aqueous solution is added with peristaltic pump, additional amount is with ZrO2It is calculated as TiO in slurry2Quality
3.0%, the concentration of zirconium sulfate aqueous solution is with ZrO2It is calculated as 95g/L；Aluminum sulfate aqueous solution is added with peristaltic pump cocurrent simultaneously, is added
Amount is with Al2O3It is calculated as TiO in slurry2The 3.0% of quality, the concentration of aluminum sulfate aqueous solution is with Al2O3It is calculated as 105g/L, zirconium sulfate is molten
The time is added as 55min in liquid and aluminum sulfate solution cocurrent, and adition process is maintained at 75 DEG C of temperature, is stirred with the revolving speed of 750r/min
It mixes；It is 7.8 that the NaOH aqueous solution for being 200g/L with concentration after adding, which adjusts slurry pH value, continues insulated and stirred curing
120min generates silicon zirconium aluminium coating titanium dioxide；
E, filtration washing: the silicon zirconium aluminium coating titanium dioxide after curing in step D is filtered with 60 DEG C of distilled water and is washed
It washs to filtrate conductivity less than 10 μ s/cm；
F, drying, crushing: to after filtration washing in step E silicon zirconium aluminium ternary coating titanium dioxide carry out expansion drying and
The titanium dioxide of silicon zirconium aluminium ternary coating is made in air-flow crushing.
The rutile titanium dioxide raw material that comparative example 1 is prepared for chloridising used in the present invention.
Titanium dioxide used in sial zirconium ternary coating titanium dioxide and comparative example 1 prepared by the embodiment of the present invention 1~4
The performance test results are shown in Table 1.
1 titanium dioxide the performance test results of table
Show the preparation method system of chloride process titanium dioxide silicon zirconium aluminium ternary coating through the invention by 1 test result of table
Standby sial zirconium ternary coating titanium dioxide has good whiteness, glossiness, water dispersible and reducing power.
Application test
By the titanium dioxide of sial zirconium ternary coating titanium dioxide and comparative example 1 prepared by above-described embodiment 1~4, answer
For detecting qualified matrix coating as test according to standard HG/T4758~2014 in water-based acrylic resin coating.Two
The additive amount of titanium oxide is the 5wt% of water-based acrylic resin coating, using water-based acrylic resin paint as this test
Reference examples 1, coating layer thickness 0.1mm can be carried out test to the weatherability of coating.At the test plate (panel) substrate of prepares coating and surface
GB/T 9271~2008 is carried out reason according to national standards, and weathering performance is tested according to GB/T 1766~2008, using people
Work accelerated ageing, Xenon light shining intensity 300W/m2, light application time 200h.Test result is as shown in table 2.
2 coating weathering performance test results of table
As the application test result of table 2 it is found that silicon zirconium aluminium ternary coating titanium dioxide prepared by the present invention, to aqueous third
The weather resistance of olefin(e) acid cold coating is significantly improved.
Claims (6)
1. a kind of preparation method of chloride process titanium dioxide silicon zirconium aluminium ternary coating, it is characterised in that: the following steps are included:
A, titanium dioxide prepared by chloridising slurry preparation: is configured to the titanium dioxide that concentration is 500~600g/L with distilled water
Titanium suspension is 9.5~10.5 with the pH value that NaOH aqueous solution adjusts tio_2 suspension, adds dispersing agent metasilicic acid
Then sodium stirs 20~30min with the revolving speed of 300~400r/min, titania slurry is made；
B, slurry is ground: the prepared titania slurry of step A is carried out 60~80min of grinding distribution with sand mill；
C, slurry heats up: titania slurry after grinding distribution being squeezed into coating tank, is warming up to 60~80 DEG C；
D, silicon zirconium aluminium coating: with two peristaltic pumps, zirconium sulfate aqueous solution and aluminum sulfate aqueous solution, zirconium sulfate water is added in cocurrent simultaneously
The additional amount of solution is with ZrO2It is calculated as TiO in slurry2The 2.0~3.0% of quality, the additional amount of aluminum sulfate aqueous solution is with Al2O3Meter
For TiO in slurry2The 2.5~3.5% of quality, adition process is maintained at 60~80 DEG C of temperature, with the revolving speed of 600~800r/min
Stirring；Adjusting slurry pH value with NaOH aqueous solution after adding is 7.0~8.0, continues insulated and stirred and cures 90~120min, raw
At silicon zirconium aluminium coating titanium dioxide；
E, washing filtration washing: is filtered to filtrate to the silicon zirconium aluminium coating titanium dioxide after curing with 50~60 DEG C of distilled water
Conductivity is less than 10 μ s/cm；
F, expansion drying and air-flow crushing, system drying, crushing: are carried out to the silicon zirconium aluminium ternary coating titanium dioxide after filtration washing
Obtain the titanium dioxide of silicon zirconium aluminium ternary coating.
2. the preparation method of chloride process titanium dioxide silicon zirconium aluminium ternary coating according to claim 1, it is characterised in that: institute
The additional amount of sodium metasilicate is stated with SiO2It is calculated as TiO in slurry2The 2.0~3.0% of quality, zirconium sulfate aqueous solution concentration is with ZrO2
It is calculated as 80~100g/L, aluminum sulfate aqueous solution concentration is with Al2O3It is calculated as 90~110g/L, sodium hydrate aqueous solution concentration is 100~
200g/L。
3. a kind of preparation method of chloride process titanium dioxide silicon zirconium aluminium ternary coating according to claim 1, feature exist
In: in the step D with peristaltic pump simultaneously cocurrent be added the addition time of zirconium sulfate aqueous solution and aluminum sulfate aqueous solution be 40~
60min。
4. a kind of preparation method of chloride process titanium dioxide silicon zirconium aluminium ternary coating according to claim 1, feature exist
In: after step B grinding in titania slurry titanium dioxide average grain diameter≤1.0 μm.
5. a kind of preparation method of chloride process titanium dioxide silicon zirconium aluminium ternary coating according to claim 1, feature exist
In: average grain diameter≤0.30 μm of obtained silicon zirconium aluminium ternary coating titanium dioxide in step F.
6. a kind of preparation method of chloride process titanium dioxide silicon zirconium aluminium ternary coating according to claim 1, feature exist
In: the titanium dioxide is the rutile titanium dioxide of chloridising preparation.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112759994A (en) * | 2021-01-22 | 2021-05-07 | 安徽天锦云节能防水科技有限公司 | Heat-insulation heat-preservation cold-insulation coating and preparation method thereof |
| CN113667348A (en) * | 2021-09-26 | 2021-11-19 | 上海摩瑟尔科学技术有限公司 | Anti-oxidation and anti-decarbonization isolation binder and preparation method thereof |
| CN114772634A (en) * | 2022-03-10 | 2022-07-22 | 贵州胜泽威化工有限公司 | Method for preparing conductive titanium dioxide |
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| US20140154413A1 (en) * | 2012-12-04 | 2014-06-05 | The National Titanium Dioxide Co. Ltd. (Cristal) | Surface treatment method for making high durability universal titanium dioxide rutile pigment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112759994A (en) * | 2021-01-22 | 2021-05-07 | 安徽天锦云节能防水科技有限公司 | Heat-insulation heat-preservation cold-insulation coating and preparation method thereof |
| CN113667348A (en) * | 2021-09-26 | 2021-11-19 | 上海摩瑟尔科学技术有限公司 | Anti-oxidation and anti-decarbonization isolation binder and preparation method thereof |
| CN114772634A (en) * | 2022-03-10 | 2022-07-22 | 贵州胜泽威化工有限公司 | Method for preparing conductive titanium dioxide |
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| CN109321002B (en) | 2020-12-04 |
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