CN111234567B - Inorganic coating process for preparing high-weather-resistance titanium dioxide - Google Patents
Inorganic coating process for preparing high-weather-resistance titanium dioxide Download PDFInfo
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- CN111234567B CN111234567B CN202010191225.5A CN202010191225A CN111234567B CN 111234567 B CN111234567 B CN 111234567B CN 202010191225 A CN202010191225 A CN 202010191225A CN 111234567 B CN111234567 B CN 111234567B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
- C09C1/3661—Coating
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3692—Combinations of treatments provided for in groups C09C1/3615 - C09C1/3684
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract
The invention belongs to the technical field of titanium dioxide production, and discloses an inorganic coating process for preparing high-weather-resistance titanium dioxide, which comprises the following steps: 1) preparing titanium dioxide slurry; 2) adding a water-soluble weak acid salt coating auxiliary agent into the titanium dioxide slurry, adjusting the temperature and the pH value of the slurry, carrying out silicon coating, adjusting the temperature and the pH value of the slurry after the silicon coating is finished, and stirring and curing; 3) adjusting the temperature and the pH value of the slurry, carrying out aluminum coating, adjusting the pH value of the slurry after the aluminum coating is finished, and stirring and curing; 4) and filtering, washing and drying the slurry to obtain a titanium dioxide product. The titanium dioxide sample prepared by the inorganic coating process has uniform silicon-aluminum coating, low acid dissolution rate, high gloss retention rate and good weather resistance.
Description
Technical Field
The invention belongs to the technical field of titanium dioxide production, and particularly relates to an inorganic coating process for preparing high-weather-resistance titanium dioxide.
Background
Titanium dioxide is titanium dioxide (TiO)2) Inorganic chemical pigments based on titanium dioxide (TiO)2) The white pigment has stable physical and chemical properties, high opacity, high whiteness and high brightness, is a white pigment with optimal performance, accounts for 80 percent of the using amount of the whole white pigment, and is widely applied to the industries of coatings, plastics, printing ink, papermaking, chemical fibers and the like.
In various application fields of titanium dioxide, weather resistance is an important application index. The weather resistance refers to the property that organic media (such as coating films and plastics) containing titanium dioxide have a series of aging phenomena such as fading, chalking, yellowing and the like under the irradiation of ultraviolet rays. The lattice defect of the titanium dioxide enables the titanium dioxide to have photocatalytic activity, thereby reducing the weather resistance of the titanium dioxide. Therefore, the improvement of the weather resistance of the titanium dioxide and the enhancement of the application performance of the pigment are important subjects of research of titanium dioxide manufacturers.
At present, there are two ways to improve the weather resistance of titanium dioxide, one is to improve the rutile type conversion rate of titanium dioxide and reduce the photocatalytic activity points of titanium dioxide. And secondly, coating one or more layers of inorganic coatings on the surface of the titanium dioxide to isolate the titanium dioxide from contacting with an organic medium. Aiming at the inorganic coating process of titanium dioxide, the inorganic coating process of titanium dioxide which is commonly adopted at home and abroad is silicon-aluminum coating or zirconium-aluminum coating. The key for improving the weather resistance of the titanium dioxide is to realize the uniform and complete coating of the inorganic coating material on the surface of the titanium dioxide.
Disclosure of Invention
In view of the above situation, the invention aims to provide an inorganic coating process for preparing high-weather-resistance titanium dioxide, wherein a silicon-aluminum film is uniformly coated on the surface of titanium dioxide by adding an inorganic coating auxiliary agent and controlling the temperature in the coating process, so that the weather resistance of the titanium dioxide is improved.
The invention provides an inorganic coating process for preparing high-weather-resistance titanium dioxide, which comprises the following steps:
1) preparing titanium dioxide slurry;
2) adding a water-soluble weak acid salt coating auxiliary agent into the titanium dioxide slurry, adjusting the temperature and the pH value of the slurry, carrying out silicon coating, adjusting the temperature and the pH value of the slurry after the silicon coating is finished, and stirring and curing;
3) adjusting the temperature and the pH value of the slurry, carrying out aluminum coating, adjusting the pH value of the slurry after the aluminum coating is finished, and stirring and curing;
4) and filtering, washing and drying the slurry to obtain a titanium dioxide product.
According to the invention, the titanium dioxide in the titanium dioxide slurry is prepared by calcining metatitanic acid in a rotary kiln, dispersing by a Raymond mill and depolymerizing by two-time sand milling. Preferably, the rutile conversion R of the titanium dioxide is greater than or equal to 99%, and the particle size of the titanium dioxide is 0.1-0.8 μm.
Preferably, the concentration of the titanium dioxide slurry is 240-320 g/L.
In the invention, the water-soluble weak acid salt coating auxiliary agent can be at least one of sodium citrate, sodium tartrate, sodium carbonate and sodium bicarbonate.
Preferably, the water-soluble weak acid salt coating auxiliary agent is sodium carbonate or sodium bicarbonate.
According to the invention, the addition amount of the water-soluble weak acid salt coating auxiliary agent is 0.2-0.6% of the mass of the titanium dioxide.
Preferably, in the step 2), the temperature of the slurry is adjusted to be 50-70 ℃, the pH value is adjusted to be 9.0-10.0, silicon coating is carried out in a mode of parallel flow of a sodium silicate solution and dilute sulfuric acid, the pH value and the temperature of the slurry are kept stable in the coating process, and homogenization is carried out for 0.5h after coating.
Preferably, the silicon coating amount is 3 to 3.5% by mass of the titanium dioxide in terms of silicon dioxide.
According to the invention, in the step 2), after the silicon coating is finished, the temperature of the slurry is adjusted to 85-95 ℃, the pH value is adjusted to 6.0-6.5, and the slurry is stirred and aged for 0.5-2.0h, preferably for 1 h.
Preferably, in the step 3), the temperature of the slurry is adjusted to 70-80 ℃ and the pH value is adjusted to 7.5-8.5, aluminum coating is carried out by adopting a parallel flow mode of a sodium metaaluminate solution and dilute sulfuric acid, the pH value and the temperature of the slurry are kept stable in the coating process, and homogenization is carried out for 0.5h after coating.
Preferably, the amount of aluminum coating is 2.5 to 3.5% by mass of titanium dioxide, calculated as aluminum oxide.
According to the invention, in the step 3), after the aluminum-clad film is finished, the pH value of the slurry is adjusted to 6.0-6.5, and the slurry is stirred and aged for 0.5-2.0h, preferably for 1 h.
Preferably, in the step 4), the washing filtrate is filtered and washed until the conductivity of the washing filtrate is less than or equal to 100 mu s/cm.
The process parameters not defined in the present invention are carried out in the conventional manner in the art, for example, dispersion by Raymond mill, sand milling, slurry preparation, etc.
Compared with the prior art, the invention has the following beneficial effects:
by adopting the silicon-aluminum coating process, the uniform coating of the silicon-aluminum coating film is realized by adding the water-soluble weak acid salt coating auxiliary agent and controlling the curing temperature of the coating, and the weather resistance of the titanium dioxide can be improved.
Drawings
FIG. 1: the contrast chart of the gloss retention of the titanium dioxide samples prepared in examples 1-4 and comparative example 1 of the invention.
FIG. 2: the contrast chart of the gloss retention of the titanium dioxide samples prepared in the embodiment 5 and the comparative examples 2 to 4 of the invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Examples 1-5 are provided to illustrate the inorganic coating process for preparing highly weatherable titanium dioxide according to the present invention.
Example 1
3 l of TiO are taken2Sanding TiO with concentration of 300g/L2Slurry, 4.05 grams of sodium carbonate solids were added, the slurry pH was adjusted to 9.0 and the slurry was heated to 60 ℃. 315mL of a solution (in SiO) at a concentration of 100g/L over 1 hour2Meter) and dilute sulfuric acid solution are added into the slurry in parallel, the pH value and the temperature are kept stable in the coating process, and then the mixture is homogenized for 30 minutes. Adjusting the pH value of the slurry to 6.0, heating the slurry to 90 ℃, and curing for 1 hour.When the temperature of the slurry is reduced to 80 ℃, the pH value of the slurry is adjusted to 8.0, and the concentration of 270mL (using Al) is 100g/L within 1 hour2O3Meter) and dilute sulfuric acid solution are added into the slurry in parallel, the temperature and the pH value are kept stable in the coating process, and then the mixture is homogenized for 30 minutes. And adjusting the pH value of the slurry to 6.0, aging for 1 hour, filtering, washing, and drying a filter cake to obtain a titanium dioxide sample 1.
Example 2
The inorganic coating process of this embodiment is the same as that of embodiment 1, except that: sodium bicarbonate is used as a coating auxiliary agent instead of sodium carbonate. To obtain titanium dioxide sample 1A.
Example 3
The inorganic coating process of this embodiment is the same as that of embodiment 1, except that: sodium citrate is adopted to replace sodium carbonate as a coating auxiliary agent. To obtain titanium dioxide sample 1B.
Example 4
The inorganic coating process of this embodiment is the same as that of embodiment 1, except that: sodium tartrate is adopted to replace sodium carbonate as a coating auxiliary agent. To obtain a titanium dioxide sample 1C.
Comparative example 1
The inorganic coating process of this comparative example is the same as example 1 except that: and no film coating auxiliary agent sodium carbonate is added. To obtain titanium dioxide sample 1D.
Example 5
3 l of TiO are taken2Sanding TiO with concentration of 300g/L2Slurry, 4.05 grams of sodium carbonate solids were added, the slurry pH was adjusted to 9.0 and the slurry was heated to 65 ℃. 315mL of a solution (in SiO) at a concentration of 100g/L over 1 hour2Meter) and dilute sulfuric acid solution are added into the slurry in parallel, the pH value and the temperature are kept stable in the coating process, and then the mixture is homogenized for 30 minutes. Adjusting the pH value of the slurry to 6.0, heating the slurry to 95 ℃, and curing for 1 hour. The temperature of the slurry was adjusted to 80 ℃, the pH of the slurry was adjusted to 8.0, and 270mL of the slurry was added (as Al) at a concentration of 100g/L over 1 hour2O3Meter) and dilute sulfuric acid solution are added into the slurry in parallel, the temperature and the pH value are kept stable in the coating process, and then the mixture is homogenized for 30 minutes. Adjusting pH of the slurry to 6.0, aging for 1 hr, and filteringWashing and drying the filter cake to obtain the titanium dioxide product. To obtain titanium dioxide sample 2.
Comparative example 2
The inorganic coating process of this comparative example is the same as example 5 except that: the temperature of silicon coating and the curing temperature of the silicon coating are both controlled to be 65 ℃. To obtain titanium dioxide sample 2A.
Comparative example 3
The inorganic coating process of this comparative example is the same as example 5 except that: the temperature of silicon coating and the curing temperature of the silicon coating are both controlled to be 95 ℃. To obtain titanium dioxide sample 2B.
Comparative example 4
The inorganic coating process of this comparative example is the same as example 5 except that: the temperature of the silicon coating is controlled to be 95 ℃, and the curing temperature of the silicon coating is controlled to be 65 ℃. To obtain titanium dioxide sample 2C.
And (3) carrying out acid dissolution rate test and xenon lamp rapid aging test on the silicon-aluminum coated titanium dioxide samples prepared in the examples and the comparative examples. The acid solubility results are shown in table 1, and the xenon lamp rapid aging test results (change of the coating light retention rate with the test time) are shown in fig. 1 and 2.
The acid solubility test method is as follows: 0.2 g of titanium dioxide was added to 10mL of 98% sulfuric acid, ultrasonically dispersed for 1 minute, and then dissolved at 175 ℃ and 180 ℃ for 1 hour. After the sample was taken out and cooled to room temperature, water was added to the volume of 100mL, the solution was filtered, 10mL of the filtrate was removed by a pipette, 10mL of 30% hydrogen peroxide solution was added, and the solution was diluted to 100mL with 10% sulfuric acid solution. After standing for 1 hour, the absorbance of the solution was measured at 400nm, and the amount of dissolved titanium dioxide was calculated with reference to a standard curve.
The quick aging test method is to prepare the titanium dioxide into the alkyd amino system coating, and a xenon lamp quick aging instrument is used for testing the light retention rate of the coating.
TABLE 1
The results of table 1, fig. 1 and fig. 2 show that the addition of the water-soluble weak acid salt coating auxiliary agent is beneficial to reducing the acid solubility of the titanium dioxide and improving the light retention rate of the titanium dioxide, that is, the water-soluble weak acid salt coating auxiliary agent is beneficial to improving the weather resistance of the titanium dioxide, and the performance of the sodium carbonate and sodium bicarbonate coating auxiliary agent is better. The process of silicon coating at a lower temperature (50-70 ℃) and silicon coating curing at a higher temperature (85-95 ℃) can reduce the acid solubility of the titanium dioxide and improve the light retention rate of the titanium dioxide, namely is beneficial to improving the weather resistance of the titanium dioxide.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the illustrated embodiments.
Claims (6)
1. An inorganic coating process for preparing high-weather-resistance titanium dioxide is characterized by comprising the following steps:
1) preparing titanium dioxide slurry;
2) adding a water-soluble weak acid salt coating auxiliary agent into the titanium dioxide slurry, adjusting the temperature and the pH value of the slurry, carrying out silicon coating, adjusting the temperature and the pH value of the slurry after the silicon coating is finished, and stirring and curing;
3) adjusting the temperature and the pH value of the slurry, carrying out aluminum coating, adjusting the pH value of the slurry after the aluminum coating is finished, and stirring and curing;
4) filtering, washing and drying the slurry to obtain a titanium dioxide product;
the water-soluble weak acid salt coating auxiliary agent is at least one of sodium citrate, sodium tartrate, sodium carbonate and sodium bicarbonate; the addition amount of the water-soluble weak acid salt coating auxiliary agent is 0.2-0.6% of the mass of the titanium dioxide;
in the step 2), adjusting the temperature of the slurry to be 50-70 ℃ and the pH value to be 9.0-10.0, carrying out silicon coating by adopting a parallel flow mode of a sodium silicate solution and dilute sulfuric acid, keeping the pH value and the temperature of the slurry stable in the coating process, and homogenizing for 0.5h after coating; the silicon coating amount is 3-3.5% of the mass of the titanium dioxide calculated by silicon dioxide; after the silicon coating is finished, the temperature of the slurry is adjusted to 85-95 ℃, the pH value is 6.0-6.5, and the slurry is stirred and cured for 0.5-2.0 h.
2. The inorganic coating process for preparing high-weatherability titanium dioxide according to claim 1, characterized in that: the rutile conversion rate R of the titanium dioxide in the titanium dioxide slurry is more than or equal to 99 percent, and the particle size of the titanium dioxide is 0.1-0.8 mu m;
the concentration of the titanium dioxide slurry is 240-320 g/L.
3. The inorganic coating process for preparing high-weatherability titanium dioxide according to claim 1, characterized in that: the water-soluble weak acid salt coating auxiliary agent is sodium carbonate or sodium bicarbonate.
4. The inorganic coating process for preparing high-weatherability titanium dioxide according to claim 1, characterized in that: in the step 3), adjusting the temperature of the slurry to 70-80 ℃ and the pH value to 7.5-8.5, performing aluminum coating in a parallel flow mode of a sodium metaaluminate solution and dilute sulfuric acid, keeping the pH value and the temperature of the slurry stable in the coating process, and homogenizing for 0.5h after coating;
calculated by alumina, the coating amount of the aluminum is 2.5 to 3.5 percent of the mass of the titanium dioxide.
5. The inorganic coating process for preparing high-weatherability titanium dioxide according to claim 1, characterized in that: in the step 3), after the aluminum-coated film is finished, the pH value of the slurry is adjusted to 6.0-6.5, and the slurry is stirred and aged for 0.5-2.0 h.
6. The inorganic coating process for preparing high-weatherability titanium dioxide according to claim 1, characterized in that: in the step 4), filtering and washing are carried out until the conductivity of the washing filtrate is less than or equal to 100 mu s/cm.
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| CN114479519A (en) * | 2021-12-28 | 2022-05-13 | 龙佰襄阳钛业有限公司 | Method for improving fluidity of titanium dioxide coating slurry |
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