CN112795208A - Preparation method of organic high-catalytic pearlescent pigment - Google Patents
Preparation method of organic high-catalytic pearlescent pigment Download PDFInfo
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- CN112795208A CN112795208A CN202011379468.8A CN202011379468A CN112795208A CN 112795208 A CN112795208 A CN 112795208A CN 202011379468 A CN202011379468 A CN 202011379468A CN 112795208 A CN112795208 A CN 112795208A
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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
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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
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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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
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/043—Drying, calcination
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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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- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention relates to the technical field of mica iron oxide preparation, in particular to a preparation method of an organic high-catalytic pearlescent pigment, which comprises the steps of putting a mica sheet, an aluminum oxide sheet, a stannic chloride solution, an iron oxide solution, a chromium oxide solution, a sodium metasilicate solution and a titanium dioxide solution into a constant-temperature pot, then sequentially adding the stannic chloride solution, the iron oxide solution, the chromium oxide solution, the stannic chloride solution, the sodium metasilicate solution and the titanium dioxide solution, and finally taking out a suspension for filtering, washing, drying, calcining and sieving. The difference between the first comparative example, the second example and the third example is that: the quality of the chromic oxide solution added in the stage of manufacturing the color development layer can influence the coverage rate of the color development layer, and the addition amount is in direct proportion to the coverage rate of the color development layer in a certain range, so that the production efficiency of the pearlescent pigment is improved to a certain extent by adding the chromic oxide solution in the production process.
Description
Technical Field
The invention relates to the technical field of mica iron oxide preparation, in particular to a preparation method of an organic high-catalytic pearlescent pigment.
Background
Pearlescent pigments are optical effect pigments, which are also called metallic non-metallic pigments because they exhibit a certain metallic luster. The pearlescent pigment has the flashing effect of metal pigment, can generate the soft color of natural pearl, can generate multi-level reflection when being irradiated by sunlight, and the reflected light interacts to present soft and dazzling or colorful luster and color. Can be widely applied to the fields of coatings, plastics, rubber, printing ink, paper, textiles, cosmetics, ornaments, artware, leather, enamel, ceramics, packaging articles, printing decoration, building materials and the like.
At present, most of pearlescent pigments used by people use organic or inorganic thin slices as base points, one or more layers of oxides are wrapped on the surfaces of the organic or inorganic thin slices, and after light is reflected, transmitted or refracted among the oxide layers, the pearlescent flashing effect is further realized.
Disclosure of Invention
The invention aims to provide a preparation method of an organic high-catalytic pearlescent pigment, which aims to solve the problem that the conventional pearlescent pigment needs to be coated with films in multiple steps in production, wherein a color development layer generally needs a long time in the process of coating the films, so that the actual production efficiency is improved.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of organic high-catalytic pearlescent pigment comprises mica flakes, aluminum oxide flakes, stannic chloride solution, ferric oxide solution, chromic oxide solution, sodium metasilicate solution and titanium dioxide solution, and comprises the following specific steps:
the method comprises the following steps: and (4) taking materials. Taking 60-80 parts of mica flakes and 60-80 parts of aluminum oxide flakes as substrates, taking 400-500 parts of ionized water, and putting the two into a constant temperature pot for mixing, wherein the temperature of the constant temperature pot is kept at 50-70 ℃;
step two: and (5) manufacturing a base film. Adjusting the temperature of the suspension in the first step to 70-80 ℃, and adding 10-30 parts of stannic chloride solution; stirring for 10-20 min, adding 50 parts of ionized water again, and stirring for 2-5 min to form a tin tetrachloride coating layer;
step three: and manufacturing a color development layer. Adjusting the temperature of the suspension in the second step to 50-60 ℃, adding 100-140 parts of ferric oxide solution and 50-100 parts of chromic oxide solution, and stirring for 10-20 minutes to form a ferric oxide solution color development layer;
step four: and manufacturing a second base film. Adjusting the temperature of the suspension liquid in the third step to 70-80 ℃, and adding 40-50 parts of stannic chloride solution; stirring for 10-20 min, adding 50 parts of ionized water again, stirring for 2-5 min, and forming a tin tetrachloride coating layer again;
step five: and manufacturing a third base layer. Adjusting the temperature of the suspension liquid in the step four to 90-100 ℃, adding 80-100 parts of sodium metasilicate solution, and stirring for 10-20 min to form a silicon dioxide coating layer;
step six: and manufacturing a protective layer. Regulating the temperature of the suspension liquid in the step five to 90-100 ℃, adding 20-30 parts of titanium dioxide solution, and stirring for 10-20 min to form a titanium dioxide protective layer;
step seven: and taking out the suspension liquid obtained in the sixth step, filtering, washing, drying, calcining at 550-600 ℃, and sieving to obtain the pearlescent pigment.
Preferably, the fatty acid is added in the step one, and the pH value is adjusted to 4.0-4.5.
Preferably, the mica flake and the aluminum oxide flake in the first step have the thickness of 0.2-2 μm and the particle size of 5-700 μm.
Preferably, the concentration of the tin tetrachloride solution in the second step and the fourth step is 80 g/L.
Preferably, the solid-liquid specific gravity of the mixed sodium metasilicate solution in the fifth step is 2: 5.
Preferably, the rotating speed of the stirring shaft in the fifth step is 200-300 r/min.
Preferably, the calcination time in the seventh step is 10-15 min.
Compared with the prior art, the invention has the beneficial effects that: under the same conditions, the color-developing layer coverage is influenced by adding the chromium oxide solution at the stage of manufacturing the color-developing layer. Under the same condition, the quality of the chromic oxide solution added in the stage of manufacturing the color development layer can influence the coverage rate of the color development layer, and the addition amount is in direct proportion to the coverage rate of the color development layer in a certain range, so that the production efficiency of the pearlescent pigment is improved to a certain extent by adding the chromic oxide solution in the production process.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
A preparation method of an organic high-catalytic pearlescent pigment comprises the following steps of preparing mica flakes, aluminum oxide flakes, a stannic chloride solution, an iron oxide solution, a chromium oxide solution, a sodium metasilicate solution and a titanium dioxide solution:
the method comprises the following steps: and (4) taking materials. Taking 60-80 parts of mica flakes and 60-80 parts of aluminum oxide flakes as substrates, taking 400-500 parts of ionized water, and putting the two into a constant temperature pot for mixing, wherein the temperature of the constant temperature pot is kept at 50-70 ℃;
step two: and (5) manufacturing a base film. Adjusting the temperature of the suspension in the first step to 70-80 ℃, and adding 10-30 parts of stannic chloride solution; stirring for 10-20 min, adding 50 parts of ionized water again, and stirring for 2-5 min to form a tin tetrachloride coating layer;
step three: and manufacturing a color development layer. Adjusting the temperature of the suspension in the second step to 50-60 ℃, adding 100-140 parts of ferric oxide solution and 50-100 parts of chromic oxide solution, and stirring for 10-20 minutes to form a ferric oxide solution color development layer;
step four: and manufacturing a second base film. Adjusting the temperature of the suspension liquid in the third step to 70-80 ℃, and adding 40-50 parts of stannic chloride solution; stirring for 10-20 min, adding 50 parts of ionized water again, stirring for 2-5 min, and forming a tin tetrachloride coating layer again;
step five: and manufacturing a third base layer. Adjusting the temperature of the suspension liquid in the step four to 90-100 ℃, adding 80-100 parts of sodium metasilicate solution, and stirring for 10-20 min to form a silicon dioxide coating layer;
step six: and manufacturing a protective layer. Regulating the temperature of the suspension liquid in the step five to 90-100 ℃, adding 20-30 parts of titanium dioxide solution, and stirring for 10-20 min to form a titanium dioxide protective layer;
step seven: and taking out the suspension liquid obtained in the sixth step, filtering, washing, drying, calcining at 550-600 ℃, and sieving to obtain the pearlescent pigment.
Further, adding fatty acid in the step one, and adjusting the pH value to 4.0-4.5.
Further, the mica sheet and the aluminum oxide sheet in the first step have the thickness of 0.2-2 μm and the particle size of 5-700 μm.
Further, the concentration of the tin tetrachloride solution in the second step and the fourth step is 80 g/L.
Further, in the fifth step, the mixed solid-liquid specific gravity of the sodium metasilicate solution is 2: 5.
furthermore, the rotating speed of the stirring shaft in the fifth step is 200-300 r/min.
Further, the calcination time in the seventh step is 10-15 min.
The first embodiment;
the method comprises the following steps: and (4) taking materials. Taking 70 parts of mica flakes and 70 parts of aluminum oxide flakes as substrates, taking 400 parts of ionized water, and putting the two into a constant temperature pot for mixing, wherein the temperature of the constant temperature pot is kept at 60 ℃;
step two: and (5) manufacturing a base film. Adjusting the temperature of the suspension in the first step to 70-80 ℃, and adding 20 parts of stannic chloride solution; stirring for 15min, adding 50 parts of ionized water again, and stirring for 5min to form a tin tetrachloride coating layer;
step three: and manufacturing a color development layer. Adjusting the temperature of the suspension in the second step to 60 ℃, adding 100 parts of ferric oxide solution and 100 parts of chromic oxide solution, stirring for 20 minutes to form a developing layer of the ferric oxide solution, wherein the coating of the developing layer of the ferric oxide solution on the detection substrate is about 12 percent
Step four: and manufacturing a second base film. Adjusting the temperature of the suspension in the third step to 80 ℃, and adding 50 parts of stannic chloride solution; stirring for 20min, adding 50 parts of ionized water again, and stirring for 5min to form a tin tetrachloride coating layer again;
step five: and manufacturing a third base layer. Adjusting the temperature of the suspension in the step four to 100 ℃, adding 80-100 parts of sodium metasilicate solution, and stirring for 10-20 min to form a silicon dioxide coating layer;
step six: and manufacturing a protective layer. Regulating the temperature of the suspension liquid in the step five to 90-100 ℃, adding 20-30 parts of titanium dioxide solution, and stirring for 10-20 min to form a titanium dioxide protective layer;
step seven: and taking out the suspension liquid obtained in the sixth step, filtering, washing, drying, calcining at 550-600 ℃, and sieving to obtain the pearlescent pigment.
And carrying out pigment detection on the finished pearlescent pigment, and then recording detection data.
The first embodiment;
the method comprises the following steps: and (4) taking materials. Taking 70 parts of mica flakes and 70 parts of aluminum oxide flakes as substrates, taking 400 parts of ionized water, and putting the two into a constant temperature pot for mixing, wherein the temperature of the constant temperature pot is kept at 50-70 ℃;
step two: and (5) manufacturing a base film. Adjusting the temperature of the suspension in the first step to 70-80 ℃, and adding 20 parts of stannic chloride solution; stirring for 15min, adding 50 parts of ionized water again, and stirring for 5min to form a tin tetrachloride coating layer;
step three: and manufacturing a color development layer. Adjusting the temperature of the suspension in the second step to 50-60 ℃, adding 100 parts of ferric oxide solution and 100 parts of chromic oxide solution, stirring for 20 minutes to form a ferric oxide solution color development layer, wherein the coating of the ferric oxide solution color development layer on the detection substrate is about 12%
Step four: and manufacturing a second base film. Adjusting the temperature of the suspension in the third step to 80 ℃, and adding 50 parts of stannic chloride solution; stirring for 20min, adding 50 parts of ionized water again, and stirring for 5min to form a tin tetrachloride coating layer again;
step five: and manufacturing a third base layer. Regulating the temperature of the suspension liquid in the step four to 90-100 ℃, adding 100 parts of sodium metasilicate solution, and stirring for 20min to form a silicon dioxide coating layer;
step six: and manufacturing a protective layer. Regulating the temperature of the suspension liquid in the step five to 90-100 ℃, adding 20 parts of titanium dioxide solution, and stirring for 10min to form a titanium dioxide protective layer;
step seven: and taking out the suspension liquid obtained in the sixth step, filtering, washing, drying, calcining at the temperature of 600 ℃, and sieving to obtain the pearlescent pigment.
And carrying out pigment detection on the finished pearlescent pigment, and then recording detection data.
Example two;
the method comprises the following steps: and (4) taking materials. Taking 70 parts of mica flakes and 70 parts of aluminum oxide flakes as substrates, taking 400 parts of ionized water, and putting the two into a constant temperature pot for mixing, wherein the temperature of the constant temperature pot is kept at 50-70 ℃;
step two: and (5) manufacturing a base film. Adjusting the temperature of the suspension in the first step to 70-80 ℃, and adding 20 parts of stannic chloride solution; stirring for 15min, adding 50 parts of ionized water again, and stirring for 5min to form a tin tetrachloride coating layer;
step three: and manufacturing a color development layer. Adjusting the temperature of the suspension in the second step to 50-60 ℃, adding 100 parts of iron oxide solution, stirring for 20 minutes to form an iron oxide solution color development layer, wherein the coating of the iron oxide solution color development layer on the detection substrate is about 6%
Step four: and manufacturing a second base film. Adjusting the temperature of the suspension in the third step to 80 ℃, and adding 50 parts of stannic chloride solution; stirring for 20min, adding 50 parts of ionized water again, and stirring for 5min to form a tin tetrachloride coating layer again;
step five: and manufacturing a third base layer. Regulating the temperature of the suspension liquid in the step four to 90-100 ℃, adding 100 parts of sodium metasilicate solution, and stirring for 20min to form a silicon dioxide coating layer;
step six: and manufacturing a protective layer. Regulating the temperature of the suspension liquid in the step five to 90-100 ℃, adding 20 parts of titanium dioxide solution, and stirring for 10min to form a titanium dioxide protective layer;
step seven: and taking out the suspension liquid obtained in the sixth step, filtering, washing, drying, calcining at the temperature of 600 ℃, and sieving to obtain the pearlescent pigment.
And carrying out pigment detection on the finished pearlescent pigment, and then recording detection data.
Example three;
the method comprises the following steps: and (4) taking materials. Taking 70 parts of mica flakes and 70 parts of aluminum oxide flakes as substrates, taking 400 parts of ionized water, and putting the two into a constant temperature pot for mixing, wherein the temperature of the constant temperature pot is kept at 50-70 ℃;
step two: and (5) manufacturing a base film. Adjusting the temperature of the suspension in the first step to 70-80 ℃, and adding 20 parts of stannic chloride solution; stirring for 15min, adding 50 parts of ionized water again, and stirring for 5min to form a tin tetrachloride coating layer;
step three: and manufacturing a color development layer. Adjusting the temperature of the suspension in the second step to 50-60 ℃, adding 100 parts of ferric oxide solution and 50 parts of chromium oxide solution, stirring for 20 minutes to form a ferric oxide solution color development layer, wherein the coating of the ferric oxide solution color development layer on the detection substrate is about 9%
Step four: and manufacturing a second base film. The temperature of the suspension in the third step was adjusted to 80 c,
step five: and manufacturing a third base layer. Regulating the temperature of the suspension liquid in the step four to 90-100 ℃, adding 100 parts of sodium metasilicate solution, and stirring for 20min to form a silicon dioxide coating layer;
step six: and manufacturing a protective layer. Regulating the temperature of the suspension liquid in the step five to 90-100 ℃, adding 20 parts of titanium dioxide solution, and stirring for 10min to form a titanium dioxide protective layer;
step seven: and taking out the suspension liquid obtained in the sixth step, filtering, washing, drying, calcining at the temperature of 600 ℃, and sieving to obtain the pearlescent pigment.
And carrying out pigment detection on the finished pearlescent pigment, and then recording detection data.
The difference between the first and second comparative examples is that: under the same conditions, the color-developing layer coverage is influenced by adding the chromium oxide solution at the stage of manufacturing the color-developing layer.
The difference between the first comparative example and the third example is that: under the same condition, the quality of the chromic oxide solution added in the stage of manufacturing the color development layer can affect the coverage rate of the color development layer, and the addition amount is in direct proportion to the coverage rate of the color development layer within a certain range.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (7)
1. A preparation method of an organic high-catalytic pearlescent pigment comprises a mica sheet, an aluminum oxide sheet, a stannic chloride solution, an iron oxide solution, a chromium oxide solution, a sodium metasilicate solution and a titanium dioxide solution, and comprises the following specific steps:
the method comprises the following steps: and (4) taking materials. Taking 60-80 parts of mica flakes and 60-80 parts of aluminum oxide flakes as substrates, taking 400-500 parts of ionized water, and putting the two into a constant temperature pot for mixing, wherein the temperature of the constant temperature pot is kept at 50-70 ℃;
step two: and (5) manufacturing a base film. Adjusting the temperature of the suspension in the first step to 70-80 ℃, and adding 10-30 parts of stannic chloride solution; stirring for 10-20 min, adding 50 parts of ionized water again, and stirring for 2-5 min to form a tin tetrachloride coating layer;
step three: and manufacturing a color development layer. Adjusting the temperature of the suspension in the second step to 50-60 ℃, adding 100-140 parts of ferric oxide solution and 50-100 parts of chromic oxide solution, and stirring for 10-20 minutes to form a ferric oxide solution color development layer;
step four: and manufacturing a second base film. Adjusting the temperature of the suspension in the third step to 70-80 ℃, and adding 40-50 parts of stannic chloride solution; stirring for 10-20 min, adding 50 parts of ionized water again, stirring for 2-5 min, and forming a tin tetrachloride coating layer again;
step five: and manufacturing a third base layer. Adjusting the temperature of the suspension liquid in the step four to 90-100 ℃, adding 80-100 parts of sodium metasilicate solution, and stirring for 10-20 min to form a silicon dioxide coating layer;
step six: and manufacturing a protective layer. Regulating the temperature of the suspension liquid in the step five to 90-100 ℃, adding 20-30 parts of titanium dioxide solution, and stirring for 10-20 min to form a titanium dioxide protective layer;
step seven: and taking out the suspension liquid obtained in the sixth step, filtering, washing, drying, calcining at 550-600 ℃, and sieving to obtain the pearlescent pigment.
2. The method for preparing organic high catalytic pearlescent pigment according to claim 1, wherein the method comprises the following steps: and adding fatty acid in the step one, and adjusting the pH value to 4.0-4.5.
3. The method for preparing organic high catalytic pearlescent pigment according to claim 1, wherein the method comprises the following steps: the mica sheet and the aluminum oxide sheet in the first step have the thickness of 0.2-2 μm and the particle size of 5-700 μm.
4. The method for preparing organic high catalytic pearlescent pigment according to claim 1, wherein: the concentration of the stannic chloride solution in the second step and the fourth step is 80 g/L.
5. The method for preparing organic high catalytic pearlescent pigment according to claim 1, wherein the method comprises the following steps: in the fifth step, the mixed solid-liquid specific gravity of the sodium metasilicate solution is 2: 5.
6. the method for preparing organic high catalytic pearlescent pigment according to claim 1, wherein the method comprises the following steps: and in the fifth step, the rotating speed of the stirring shaft is 200-300 r/min.
7. The method for preparing organic high catalytic pearlescent pigment according to claim 1, wherein the method comprises the following steps: and the calcination time in the seventh step is 10-15 min.
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