CN111393875A - Preparation method of titanium dioxide coated rare earth base pearlescent pigment - Google Patents
Preparation method of titanium dioxide coated rare earth base pearlescent pigment Download PDFInfo
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- CN111393875A CN111393875A CN202010233800.3A CN202010233800A CN111393875A CN 111393875 A CN111393875 A CN 111393875A CN 202010233800 A CN202010233800 A CN 202010233800A CN 111393875 A CN111393875 A CN 111393875A
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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
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
- C09C1/0021—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a core coated with only one layer having a high or low refractive index
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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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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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
- C09C2220/00—Methods of preparing the interference pigments
- C09C2220/10—Wet methods, e.g. co-precipitation
- C09C2220/103—Wet methods, e.g. co-precipitation comprising a drying or calcination step after applying each layer
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Abstract
The invention relates to a preparation method of titanium dioxide coated rare earth based pearlescent pigment, which comprises the following experimental steps of dropwise adding water solution of light rare earth salt with the concentration of 0.1-2.0 mol/L into alkaline solution with the concentration of 0.01-1.0 mol/L, reacting for 0.5-48h at the stirring speed of 0-3000r/min and the temperature of 0-40 ℃, aging for 0.5-24h to obtain rare earth sheet materials, obtaining sheet materials with different particle sizes by changing conditions, treating the sheet materials for 0.5-48h at the temperature of 0-50 ℃ through a surfactant, adding the treated sheet materials into a solution containing a titanium compound, slowly dropwise adding an alkaline precipitator, obtaining an intermediate product at the stirring speed of 100 r/min and the temperature of 0-40 ℃, obtaining the intermediate product at the time of 2-24h, obtaining the intermediate product with different coating thicknesses by changing conditions, filtering, washing, drying and calcining the intermediate product to obtain a final product, simplifying the process, reducing the synthesis temperature, reducing the energy consumption of the synthesis process, and realizing the simple synthesis of the titanium dioxide coated rare earth based pearlescent pigment.
Description
Technical Field
The invention relates to the field of pearlescent pigments, in particular to a preparation method of a titanium dioxide coated rare earth-based pearlescent pigment.
Background
The pearlescent pigment is used as a special effect pigment and is mainly applied to the fields of plastics, cosmetics, coatings, printing ink and the like. The pearlescent pigment is used for imitating the effect of naturally existing pearls, and is artificially synthesized as a special effect pigment with high added value. The traditional pearlescent pigment products are all made of natural mica, synthetic mica and Al2O3、SiO2The materials are base materials of pearlescent pigments, and one or more layers of TiO are coated on the surface of the base materials2To improve the pearl effect. Rare earth has the name of 'industrial vitamin', and because the rare earth has excellent magneto-optical electrical properties, the rare earth is also introduced into the field of pearlescent pigments, and generally has the functions of enabling the pearlescent pigments to have special functions of color, reflecting ultraviolet rays, absorbing infrared rays and the like. The method has wide application in various industries, particularly high and new technology industries, and comprises the field of pearlescent materials. Although pearlescent pigments containing rare earths have excellent properties, the preparation process is generally complicated. For example, CN101693790A describes a composite mica cerium titanium pearlescent pigment and a preparation method thereof, wherein a layer of cerium dioxide is coated on the surface of mica, and a layer of titanium dioxide is coated on the surface of cerium dioxide.
Disclosure of Invention
The technical problems to be solved by the invention are as follows:
the invention provides a pearlescent pigment containing rare earth, which is prepared by using a rare earth sheet material as a matrix and titanium dioxide as a coating layer through one-step coating.
The technical scheme adopted by the invention is as follows:
a preparation method of titanium dioxide coated rare earth base pearlescent pigment comprises the following experimental steps:
(1) dropwise adding the water solution of the light rare earth salt with the concentration of 0.1-2.0 mol/L into the alkaline solution with the concentration of 0.01-1.0 mol/L;
(2) reacting for 0.5-48h at the stirring speed of 0-3000r/min and the temperature of 0-40 ℃, and then aging for 0.5-24h to obtain a rare earth sheet material, wherein the sheet materials with different particle sizes can be obtained by changing the conditions;
(3) treating the flaky material for 0.5-48h at the temperature of 0-50 ℃ by using a surfactant, adding the treated flaky material into a solution containing a titanium compound, slowly dropwise adding an alkaline precipitator, and obtaining an intermediate product at the stirring speed of 100-2000 r/min, the temperature of 0-40 ℃ and the time of 2-24 h;
(4) intermediate products with different coating thicknesses can be obtained by changing conditions. The intermediate product is filtered, washed, dried and calcined to obtain the final product.
The water solution of the light rare earth salt is chloride solution containing one or more of L a, Ce, Pr and Nd.
The water solution of the light rare earth salt is a nitrate solution containing one or more of L a, Ce, Pr and Nd.
The surfactant is a high molecular compound containing carbonyl, hydroxyl and carboxyl.
The surfactant is polyethylene glycol, citric acid or polyvinylpyrrolidone.
The solution containing titanium compound is solution with tetrabutyl titanate or titanium tetrachloride as solute and water, methanol, ethanol, acetonitrile or acetone as solvent.
The alkaline precipitator is ammonia water, sodium carbonate, sodium hydroxide or urea.
The invention has the beneficial effects that:
the method has the advantages of simple process flow, lower synthesis temperature, short reaction time, reduced energy consumption and realization of simple synthesis of the titanium dioxide coated rare earth-based pearlescent pigment.
Detailed Description
Example 1
50ml of 0.5 mol/L cerium nitrate aqueous solution is dripped into 450ml of 0.15 mol/L ammonium bicarbonate aqueous solution, the mixture reacts for 6 hours at 25 ℃ under the stirring speed of 1000r/min, and then is aged for 6 hours to obtain a rare earth sheet material, the sheet material is treated for 12 hours at 25 ℃ by polyethylene glycol, 100g of the treated sheet material is added into a mixed solution of 500ml of ethanol and 1500ml of water containing 10ml of titanium tetrachloride, 5ml of ammonia water is slowly reacted for 6 hours at 500r/min and 25 ℃ to obtain an intermediate product, and the intermediate product is filtered, washed by water for 3 times, dried for 12 hours at 60 ℃ and calcined at 600 ℃ to obtain the yellow pearlescent pigment.
Example 2
50ml of 0.5 mol/L cerium praseodymium nitrate mixed solution is dropwise added into 450ml of 0.15 mol/L ammonium bicarbonate aqueous solution (wherein the molar ratio of cerium to praseodymium is mCe/Pr =9: 1), the mixture reacts for 6 hours at 25 ℃ at the stirring speed of 1000r/min, then is aged for 6 hours to obtain rare earth sheet material, the sheet material is treated for 12 hours at 25 ℃ by polyethylene glycol, 100g of the treated sheet material is added into the mixture of 500ml of ethanol and 1500ml of water containing 10ml of titanium tetrachloride, 5ml of ammonia water is slowly dropped, the mixture reacts for 6 hours at 25 ℃ at 500r/min, and an intermediate product is obtained, and the intermediate product is filtered, washed by water for 3 times, dried for 12 hours at 60 ℃ and calcined at 600 ℃ to obtain the dark red pearlescent pigment.
Example 3
50ml of 0.1 mol/L mol/cerium chloride aqueous solution is dripped into 450ml of 0.03 mol/L mol/ammonium bicarbonate aqueous solution, the mixture is stirred at the speed of 1000r/min and is reacted for 6 hours at the temperature of 25 ℃, then the mixture is aged for 6 hours to obtain a rare earth sheet material, the sheet material is treated for 12 hours at the temperature of 25 ℃ by polyethylene glycol, 100g of the treated sheet material is added into a mixed solution of 500ml of ethanol and 1500ml of water containing 10ml of titanium tetrachloride, 5ml of ammonia water is slowly reacted for 6 hours at the temperature of 500r/min and 25 ℃ to obtain an intermediate product, and the intermediate product is filtered, washed by water for 3 times, dried for 12 hours at the temperature of 60 ℃ and calcined at the temperature of 600 ℃ to obtain the yellow pearlescent pigment.
Example 4
50ml of 2 mol/L mol/praseodymium nitrate aqueous solution is dropwise added into 450ml of 0.6 mol/L sodium carbonate aqueous solution, the mixture is stirred at the speed of 1000r/min and is reacted for 6 hours at 25 ℃, then the mixture is aged for 6 hours to obtain a rare earth sheet material, the sheet material is treated for 12 hours at 25 ℃ by polyethylene glycol, 100g of the treated sheet material is added into a mixed solution of 500ml of ethanol and 1500ml of water containing 10ml of titanium tetrachloride, 5ml of ammonia water is slowly dropped into the mixed solution, and the mixed solution is reacted for 6 hours at 500r/min and 25 ℃ to obtain an intermediate product, and the intermediate product is filtered, washed by water for 3 times, dried for 12 hours at 60 ℃ and calcined at 600 ℃ to obtain the sepia pearlescent pigment.
Example 5
50ml of 0.5 mol/L lanthanum chloride aqueous solution is dripped into 450ml of 0.15 mol/L ammonia aqueous solution, the mixture is stirred at the speed of 0r/min and reacted at the temperature of 0 ℃ for 0.5 hour, and then aged for 6 hours to obtain a rare earth sheet material, the sheet material is treated by polyethylene glycol at the temperature of 25 ℃ for 12 hours, 100g of the treated sheet material is added into a mixed solution of 500ml of ethanol and 1500ml of water containing 10ml of titanium tetrachloride, 5ml of ammonia water is slowly reacted at the temperature of 500r/min and 25 ℃ for 6 hours to obtain an intermediate product, and the intermediate product is filtered, washed by water for 3 times, dried at the temperature of 60 ℃ for 12 hours, and calcined at the temperature of 600 ℃ to obtain the white pearlescent pigment.
Example 6
50ml of 0.5 mol/L cerium nitrate aqueous solution is dripped into 450ml of 0.15 mol/L urea aqueous solution, the mixture is stirred at 3000r/min and reacted at 40 ℃ for 24 hours, and then aged for 24 hours to obtain a rare earth sheet material, the sheet material is treated by polyethylene glycol at 25 ℃ for 12 hours, 100g of the treated sheet material is added into a mixed solution of 500ml of ethanol and 1500ml of water containing 10ml of titanium tetrachloride, 5ml of ammonia water is slowly dripped into the mixed solution, and the mixed solution is reacted at 500r/min and 25 ℃ for 6 hours to obtain an intermediate product, and the intermediate product is filtered, washed by water for 3 times, dried at 60 ℃ for 12 hours and calcined at 600 ℃ to obtain the yellow pearlescent pigment.
Example 7
50ml of 0.5 mol/L mol/cerium nitrate aqueous solution is dripped into 450ml of 0.15 mol/L mol/sodium hydroxide aqueous solution, the mixture is stirred at the speed of 1000r/min and reacted at 25 ℃ for 6 hours, and then aged for 0.5 hour to obtain a rare earth sheet material, the sheet material is treated by polyethylene glycol at 0 ℃ for 48 hours, 100g of the treated sheet material is added into a mixed solution of 500ml of ethanol and 1500ml of water containing 10ml of titanium tetrachloride, 5ml of ammonia water is slowly dripped into the mixed solution, and the mixed solution is reacted at 500r/min and 25 ℃ for 6 hours to obtain an intermediate product, and the intermediate product is filtered, washed by water for 3 times, dried at 60 ℃ for 12 hours and calcined at 600 ℃ to obtain the yellow pearlescent pigment.
Example 8
50ml of 0.5 mol/L cerium nitrate aqueous solution is dripped into 450ml of 0.15 mol/L ammonium bicarbonate aqueous solution, the mixture is stirred at the speed of 1000r/min and reacted at the temperature of 25 ℃ for 6 hours, and then aged for 0.5 hour to obtain a rare earth sheet material, the sheet material is treated by polyethylene glycol at the temperature of 50 ℃ for 0.5 hour, 100g of the treated sheet material is added into a mixed solution of 500ml of ethanol and 1500ml of water containing 10ml of titanium tetrachloride, 5ml of ammonia water is slowly dripped into the mixed solution, and the mixed solution is reacted at the temperature of 500r/min and 25 ℃ for 6 hours to obtain an intermediate product, and the intermediate product is filtered, washed by water for 3 times, dried at the temperature of 60 ℃ for 12 hours and calcined at the temperature of 600 ℃ to obtain the yellow pearlescent.
Example 9
50ml of 0.5 mol/L cerium nitrate aqueous solution is dripped into 450ml of 0.15 mol/L ammonium bicarbonate aqueous solution, the mixture is stirred at the speed of 1000r/min and reacted at 25 ℃ for 6 hours, and then aged for 6 hours to obtain a rare earth sheet material, the sheet material is treated by polyvinylpyrrolidone at 25 ℃ for 12 hours, 100g of the treated sheet material is added into a mixed solution of 500ml of ethanol and 1500ml of water containing 10ml of titanium tetrachloride, 5ml of ammonia water is slowly dripped into the mixed solution, and the mixed solution is reacted at 500r/min and 25 ℃ for 6 hours to obtain an intermediate product, and the intermediate product is filtered, washed by water for 3 times, dried at 60 ℃ for 12 hours and calcined at 600 ℃ to obtain the yellow pearlescent pigment.
Example 10
50ml of 0.5 mol/L cerium nitrate aqueous solution is dripped into 450ml of 0.15 mol/L ammonium bicarbonate aqueous solution, the mixture is stirred at the speed of 1000r/min and reacted at 25 ℃ for 6 hours, and then aged for 6 hours to obtain a rare earth sheet material, the sheet material is treated by polyvinylpyrrolidone at 25 ℃ for 12 hours, 100g of the treated sheet material is added into a mixed solution of 10ml of tetrabutyl titanate, 500ml of ethanol and 1500ml of water, 5ml of ammonia water is slowly dripped into the mixed solution, the mixed solution is reacted at 500r/min and 25 ℃ for 6 hours to obtain an intermediate product, and the intermediate product is filtered, washed by water for 3 times, dried at 60 ℃ for 12 hours and calcined at 600 ℃ to obtain the pearlescent pigment.
Example 11
50ml of 0.5 mol/L cerium nitrate aqueous solution is dripped into 450ml of 0.15 mol/L ammonium bicarbonate aqueous solution, the mixture reacts for 6 hours at 25 ℃ under the stirring speed of 1000r/min, and then is aged for 6 hours to obtain a rare earth sheet material, the sheet material is treated for 12 hours at 25 ℃ by polyethylene glycol, 100g of the treated sheet material is added into a mixed solution of 500ml acetonitrile and 1500ml water containing 10ml titanium tetrachloride, 5ml ammonia water is slowly added, the mixture reacts for 2 hours at 0 ℃ and 2000 r/min to obtain an intermediate product, and the intermediate product is filtered, washed by water for 3 times, dried for 12 hours at 60 ℃ and calcined at 600 ℃ to obtain yellow pearlescent pigment.
Example 12
50ml of 0.5 mol/L mol/cerium nitrate aqueous solution is dripped into 450ml of 0.15 mol/L mol/ammonium bicarbonate aqueous solution, the mixture is stirred at the speed of 1000r/min and reacted at 25 ℃ for 6 hours, and then aged for 6 hours to obtain a rare earth sheet material, the sheet material is treated by citric acid at 25 ℃ for 12 hours, 100g of the treated sheet material is added into a mixed solution of 500ml of water and 1500ml of water containing 10ml of titanium tetrachloride, 5ml of ammonia water is slowly reacted at 100 r/min and 40 ℃ for 24 hours to obtain an intermediate product, and the intermediate product is filtered, washed by water for 3 times, dried at 60 ℃ for 12 hours and calcined at 600 ℃ to obtain the yellow pearlescent pigment.
Claims (7)
1. The preparation method of the titanium dioxide coated rare earth base pearlescent pigment is characterized by comprising the following experimental steps:
(1) dropwise adding the water solution of the light rare earth salt with the concentration of 0.1-2.0 mol/L into the alkaline solution with the concentration of 0.01-1.0 mol/L;
(2) reacting for 0.5-48h at the stirring speed of 0-3000r/min and the temperature of 0-40 ℃, and then aging for 0.5-24h to obtain a rare earth sheet material, wherein the sheet materials with different particle sizes can be obtained by changing the conditions;
(3) treating the flaky material for 0.5-48h at the temperature of 0-50 ℃ by using a surfactant, adding the treated flaky material into a solution containing a titanium compound, slowly dropwise adding an alkaline precipitator, and obtaining an intermediate product at the stirring speed of 100-2000 r/min, the temperature of 0-40 ℃ and the time of 2-24 h;
(4) intermediate products with different coating thicknesses can be obtained by changing conditions; the intermediate product is filtered, washed, dried and calcined to obtain the final product.
2. The preparation method according to claim 1, wherein the aqueous solution of the light rare earth salt is a chloride solution containing L a, Ce, Pr or Nd.
3. The preparation method according to claim 1, wherein the aqueous solution of the light rare earth salt is a nitrate solution containing one or more of L a, Ce, Pr and Nd.
4. The method of claim 1, wherein: the surfactant is a high molecular compound containing carbonyl, hydroxyl and carboxyl.
5. The production method according to claim 1 or 4, characterized in that: the surfactant is polyethylene glycol, citric acid or polyvinylpyrrolidone.
6. The method of claim 1, wherein: the solution containing titanium compound is solution with tetrabutyl titanate or titanium tetrachloride as solute and water, methanol, ethanol, acetonitrile or acetone as solvent.
7. The method of claim 1, wherein: the alkaline precipitator is ammonia water, sodium carbonate, sodium hydroxide or urea.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115873423A (en) * | 2022-12-29 | 2023-03-31 | 贺州学院 | Method for preparing modified calcium carbonate powder by using tetrabutyl titanate |
| CN117732420A (en) * | 2023-12-20 | 2024-03-22 | 蔚孚科技(丽水)有限公司 | Flaky porous defluorination adsorbent, and preparation method and application thereof |
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