CN109401361B - Preparation method of white inorganic ceramic pigment with pyrochlore structure - Google Patents

Preparation method of white inorganic ceramic pigment with pyrochlore structure Download PDF

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CN109401361B
CN109401361B CN201811307677.4A CN201811307677A CN109401361B CN 109401361 B CN109401361 B CN 109401361B CN 201811307677 A CN201811307677 A CN 201811307677A CN 109401361 B CN109401361 B CN 109401361B
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dissolving
ceramic pigment
nitrate
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inorganic ceramic
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CN109401361A (en
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符静
梅婉婉
杨慧
张瑞珠
仝玉萍
马军涛
王静
靳丽辉
张海龙
公静利
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Zhengzhou Chenggong University Of Finance And Economics
North China University of Water Resources and Electric Power
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Zhengzhou Chenggong University Of Finance And Economics
North China University of Water Resources and Electric Power
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    • 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
    • C09C1/0009—Pigments for ceramics
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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Abstract

The invention discloses a preparation method of a white inorganic ceramic pigment with a pyrochlore structure, wherein the white inorganic ceramic pigment has Y2Ce2‑xBaxO7Wherein X is more than or equal to 0.00 and less than or equal to 0.50, and the preparation method comprises the following steps: respectively dissolving corresponding yttrium nitrate, cerium nitrate and barium nitrate in distilled water according to the molar ratio of Y, Ce to Ba to obtain a mixed solution; adding into glycine water solution; stirring for more than 1h, and then burning and concentrating at 120 ℃ to obtain precursor powder; calcining the mixture for 4 hours at 500-900 ℃ by using a muffle furnace to obtain a white ceramic pigment with a pyrochlore structure; the preparation method of the invention saves energy and time, the raw materials are easy to obtain, and the obtained product has good ion dispersibility, uniform particle size distribution, no toxicity and no radioactivity; the synthesis temperature is low, the process is simple and controllable, and the method is suitable for large-scale production.

Description

Preparation method of white inorganic ceramic pigment with pyrochlore structure
Technical Field
The invention belongs to the technical field of ceramic pigments, and particularly relates to a preparation method of a white inorganic ceramic pigment with a pyrochlore structure.
Background
White is a color that encompasses all colors of light in the spectrum and is generally considered "colorless" (but the opposite of black, which is colorless), with the highest lightness and zero hue. The light of the three primary colors in the spectrum can be: the red, blue and green are mixed according to a certain proportion to obtain white light. The mixture of all visible light in the spectrum is also white light. White pigments are the most important single class of pigments, since white is of significant importance in terms of color, while the application of white pigments is required to obtain many other colors and light shades. It is known that the material has excellent performance compared with the conventional material when the size of the material is reduced to nanometer level. Although other processes, such as liquid phase, precipitation, sol-gel, etc., are being explored to reduce the cost of pigment synthesis and improve the synthesis efficiency. However, these methods have problems of high production cost, complex process, etc. compared with the solid-solid sintering method, so that they cannot be popularized and applied in industrial production. Therefore, a green synthesis method is required, and a high-performance white nano pigment with small size, good dispersibility and uniform particle size distribution is imperatively obtained in a relatively mild environment.
Doping in a crystal generally means the purposeful incorporation of small amounts of other elements or compounds into such a material or matrix in order to improve the properties of the material or substance. Doping can produce specific electrical, magnetic and optical properties to the material and the matrix, thereby having specific value or application.
The patent with application number 201210188421.2 discloses a white pigment and a manufacturing process thereof, belonging to the field of wet production of white pigments. The present invention uses wollastonite powder as base material, and is matched with aluminium hydroxide gel and titanium dioxide, under the action of aluminium hydroxide gel the wollastonite powder surface can be formed into adhesive film, and the titanium dioxide can be used for making chemical film-coating treatment of wollastonite powder adhesive film.
Disclosure of Invention
In view of the above technical problems, the present invention provides a method for preparing a pyrochlore-structured white inorganic ceramic pigment having high chemical stability.
The technical scheme of the invention is as follows: a method for preparing a pyrochlore-structured white inorganic ceramic pigment having Y2Ce2-xBaxO7Wherein X is more than or equal to 0.00 and less than or equal to 0.50;the preparation method of the white inorganic ceramic pigment comprises the following steps:
1) respectively dissolving corresponding yttrium nitrate, cerium nitrate and barium nitrate in distilled water on a dissolving device according to the molar ratio of Y, Ce to Ba to obtain a mixed solution;
2) adding the mixed solution obtained in the step 1) into an aqueous solution of glycine;
3) stirring the mixed solution obtained in the step 2) for 1-10 hours at 60 ℃ by using a magnetic stirrer, and then burning and concentrating at 120 ℃ to obtain precursor powder;
4) and finally, calcining the precursor powder obtained in the step 3) by using a muffle furnace at the calcining temperature of 500-900 ℃ for 2-4 hours to obtain the white ceramic pigment with the pyrochlore structure.
Further, the white inorganic ceramic pigment has Y2Ce2-xBaxO7Wherein X is more than or equal to 0.25 and less than or equal to 0.30.
Further, in the step 1), yttrium nitrate, cerium nitrate and barium nitrate are dissolved in distilled water according to the sequence of dissolving barium nitrate, cerium nitrate and finally yttrium nitrate, and yttrium nitrate, cerium nitrate and barium nitrate are dissolved in batches, so that the respective stability is effectively ensured not to be influenced.
Further, the stirring speed in the step 3) is 80r/min-100r/min, which is more beneficial to obtaining fluffy precursor powder in the later period.
Further, stirring the mixed solution in the step 3) for 1.5-2 hours; when the reaction time is less than 1 hour, the product cannot be subjected to sufficient diffusion reaction, so that the phase of the product is not uniform, and the excessive reaction time can cause resource waste and increase the cost.
Further, the step 4) is carried out early preheating before calcination, specifically: putting the precursor powder into a muffle furnace, heating for the first time, heating to 300 ℃ at a heating rate of 5 ℃/min, and then preserving heat for 30-45 min; then adding the mixture to 500-900 ℃ at the heating rate of 20 ℃/min for calcining; preheating is effective to stabilize chemical properties, resulting in the formation of a single stable solid solution during later calcination.
Preferably, the calcination temperature in step 4) is 900 ℃.
Preferably, the calcination time in the step 4) is 3-4 h.
Further, the dissolving device in the step 1) comprises a base, a buffer tank, an oscillating device and a condensing device, wherein the buffer tank is arranged on the base through a support rod, and the oscillating device is arranged on the base and is positioned below the buffer tank; the buffer tank comprises a normal-temperature dissolution cavity and a low-temperature dissolution cavity, a liquid outlet is formed in the lower end of the buffer tank, a first dissolution bottle is arranged in the normal-temperature dissolution cavity, a second dissolution bottle is arranged in the low-temperature dissolution cavity, the condensing device is arranged in the low-temperature dissolution cavity and is positioned below the second dissolution bottle, the first dissolution bottle and the second dissolution bottle are respectively connected with the liquid outlet through connecting pipes, and a first valve and a second valve are respectively arranged at the joints; the outer side walls of the normal-temperature dissolving cavity and the low-temperature dissolving cavity are provided with a first valve switch and a second valve switch which correspond to the first valve and the second valve, and the side wall of the buffer box is provided with a control panel of a condensing device; the oscillating device comprises an oscillating motor, an oscillating connecting rod and a clamping seat, the oscillating motor provides power for the oscillating connecting rod, the clamping seat is arranged at the upper end of the oscillating connecting rod, a placing groove is arranged on the clamping seat and is positioned right below the liquid outlet, and the placing groove is used for placing a dissolving beaker; and in the dissolving process, buffering and dissolving barium nitrate and cerium nitrate in a first dissolving bottle, buffering and dissolving yttrium nitrate in a second dissolving bottle at a low temperature, and finally mixing and dissolving the dissolving solution in a dissolving beaker.
Furthermore, the temperature of the condensing device is set to be 2-5 ℃, and the chemical property of the yttrium nitrate has better stability at the temperature of 2-5 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. the white inorganic pigment has pure color, is doped with ions to enter a pyrochlore structure to form a single stable solid solution, is difficult to dissolve out, and has the advantages of good thermal stability and good chemical stability;
2. the product of the invention does not contain toxic elements such as lead, chromium and the like, and is green and environment-friendly;
3. the preparation method is simple, raw materials are easy to obtain, the obtained product has good particle dispersibility, uniform particle size distribution, low synthesis temperature and simple and controllable process, and is suitable for large-scale production.
Drawings
FIG. 1 is Y of a pyrochlore-structured white inorganic pigment of the invention2Ce2-xBaxO7Wherein X is 0, 0.05, 0.10, 0.15, 0.20, 0.30, 0.5, the abscissa is diffraction angle, and the ordinate is diffraction intensity;
FIG. 2 is Y of a white ceramic pigment having a pyrochlore structure at different temperatures2Ce2-xBaxO7XRD pattern of the powder;
FIG. 3 is Y of a pyrochlore-structured white ceramic pigment2Ce2-xBaxO7EDS plot of powder when X is 0.3;
FIG. 4 is a schematic view of the dissolving apparatus of the present invention;
fig. 5 is a sectional view of the dissolving apparatus of the present invention.
The device comprises a buffer tank 1, a normal-temperature dissolving cavity 11, a dissolving bottle I110, a valve switch I111, a low-temperature dissolving cavity 12, a dissolving bottle II 120, a valve switch II 121, a liquid outlet 13, a vibration device 2, an oscillation motor 21, a swing connecting rod 22, a clamping seat 23, a condensation device 3 and a control panel 31.
Detailed Description
Example 1:
a method for preparing a pyrochlore-structured white inorganic ceramic pigment having Y2Ce2-xBaxO7Wherein X is more than or equal to 0.00 and less than or equal to 0.50; the preparation method of the white inorganic ceramic pigment comprises the following steps:
1) dissolving 7.66g of yttrium nitrate and 8.68g of cerium nitrate in 100ml of water on a dissolving device, and stirring to obtain a solution A; dissolving 8.68g of cerium nitrate in a first dissolving bottle 110 through normal-temperature buffering, dissolving 7.66g of yttrium nitrate in a second dissolving bottle 120 through low-temperature buffering, and mixing the solutions in the first dissolving bottle 110 and the second dissolving bottle 120 in a dissolving beaker on a placing groove through a liquid outlet 13 to obtain a solution A; the water put in the first dissolving bottle 110, the second dissolving bottle 120 and the dissolving beaker is respectively 40ml, 40ml and 20ml in advance; dissolving cerium nitrate and yttrium nitrate, putting the solution in the first dissolving bottle 110 into a dissolving beaker, and putting the solution in the second dissolving bottle 120 into the dissolving beaker;
2) dissolving 6.01g of glycine into 50ml of water to obtain a solution B, pouring the solution A into the solution B, and stirring at 60 ℃ to obtain a clear solution C;
3) stirring for 2 hours at the speed of 100r/min by utilizing ultrasonic oscillation, and then concentrating and burning at the temperature of 120 ℃ to generate loose powder, namely a precursor;
4) putting the precursor powder into a muffle furnace, heating for the first time, heating to 300 ℃ at a heating rate of 5 ℃/min, and then preserving heat for 30 min; then adding the mixture to 900 ℃ at the heating rate of 20 ℃/min for calcining; calcining at 900 deg.C for 3h, and grinding again to obtain final sample Y2Ce2O7。
Example 2:
different from example 1, 7.66g of yttrium nitrate, 8.47g of cerium nitrate and 0.13g of barium nitrate were dissolved in 100ml of water and stirred to obtain a solution A; processing to obtain final sample Y2Ce1.95Ba0.05O7。
Wherein the stirring speed in the step 3) is 80r/min, the stirring time is 1.5h, the calcining temperature in the step 4) is 500 ℃, and the calcining time is 4 h.
Dissolving 8.47g of cerium nitrate and 0.13g of barium nitrate in a first dissolving bottle 110 through normal-temperature buffering, dissolving 7.66g of yttrium nitrate in a second dissolving bottle 120 through low-temperature buffering, and mixing the solutions in the first dissolving bottle 110 and the second dissolving bottle 120 into a dissolving beaker on a placing groove through a liquid outlet 13 to obtain a solution A; dissolving barium nitrate, cerium nitrate and yttrium nitrate in sequence, putting the solution in the first dissolving bottle 110 into a dissolving beaker, and putting the solution in the second dissolving bottle 120 into the dissolving beaker.
Example 3:
different from embodiment 1Dissolving 7.66g of yttrium nitrate, 8.25g of cerium nitrate and 0.26g of barium nitrate in 100ml of water, and stirring to obtain a solution A; processing to obtain final sample Y2Ce1.9Ba0.1O7。
Wherein the stirring speed in the step 3) is 90r/min, the stirring time is 1h, the calcining temperature in the step 4) is 600 ℃, and the calcining time is 4 h.
Dissolving 8.25g of cerium nitrate and 0.26g of barium nitrate in a first dissolving bottle 110 through normal-temperature buffering, dissolving 7.66g of yttrium nitrate in a second dissolving bottle 120 through low-temperature buffering, and mixing the solutions in the first dissolving bottle 110 and the second dissolving bottle 120 into a dissolving beaker on a placing groove through a liquid outlet 13 to obtain a solution A; dissolving barium nitrate, cerium nitrate and yttrium nitrate in sequence, putting the solution in the first dissolving bottle 110 into a dissolving beaker, and putting the solution in the second dissolving bottle 120 into the dissolving beaker.
Example 4:
different from example 1, 7.66g of yttrium nitrate, 8.03g of cerium nitrate and 0.39g of barium nitrate were dissolved in 100ml of water and stirred to obtain a solution A; processing to obtain final sample Y2Ce1.85Ba0.15O7。
Wherein the stirring time of the step 3) is 5 hours, the calcining temperature in the step 4) is 700 ℃, and the calcining time is 4 hours.
Wherein, 8.03g of cerium nitrate and 0.39g of barium nitrate are dissolved in a first dissolving bottle 110 through normal temperature buffering, 7.66g of yttrium nitrate is dissolved in a second dissolving bottle 120 through low temperature buffering, and then the solutions in the first dissolving bottle 110 and the second dissolving bottle 120 are mixed in a dissolving beaker on a placing groove through a liquid outlet 13 to obtain a solution A; dissolving barium nitrate, cerium nitrate and yttrium nitrate in sequence, putting the solution in the first dissolving bottle 110 into a dissolving beaker, and putting the solution in the second dissolving bottle 120 into the dissolving beaker.
Example 5:
in a difference from example 1, 7.66g of yttrium nitrate, 7.82g of cerium nitrate and 0.53g of barium nitrate were dissolved in 100ml of water and stirred to obtain a solutionA; processing to obtain final sample Y2Ce1.8Ba0.2O7。
Wherein the stirring time of the step 3) is 10 hours, the calcining temperature in the step 4) is 800 ℃, and the calcining time is 3 hours.
Wherein, 7.82g of cerium nitrate and 0.53g of barium nitrate are dissolved in a first dissolving bottle 110 through normal temperature buffering, 7.66g of yttrium nitrate is dissolved in a second dissolving bottle 120 through low temperature buffering, and then the solutions in the first dissolving bottle 110 and the second dissolving bottle 120 are mixed in a dissolving beaker on a placing groove through a liquid outlet 13 to obtain a solution A; dissolving barium nitrate, cerium nitrate and yttrium nitrate in sequence, putting the solution in the first dissolving bottle 110 into a dissolving beaker, and putting the solution in the second dissolving bottle 120 into the dissolving beaker.
Example 6:
different from example 1, 7.66g of yttrium nitrate, 7.38g of cerium nitrate and 0.79g of barium nitrate were dissolved in 100ml of water and stirred to obtain a solution A; processing to obtain final sample Y2Ce1.7Ba0.3O7。
Wherein, the stirring time in the step 3) is 10h, and the calcining time in the step 4) is 2 h.
Wherein, 7.38g of cerium nitrate and 0.79g of barium nitrate are dissolved in a first dissolving bottle 110 through normal temperature buffering, 7.66g of yttrium nitrate is dissolved in a second dissolving bottle 120 through low temperature buffering, and then the solutions in the first dissolving bottle 110 and the second dissolving bottle 120 are mixed in a dissolving beaker on a placing groove through a liquid outlet 13 to obtain a solution A; dissolving barium nitrate, cerium nitrate and yttrium nitrate in sequence, putting the solution in the first dissolving bottle 110 into a dissolving beaker, and putting the solution in the second dissolving bottle 120 into the dissolving beaker.
Example 7:
different from example 1, 7.66g of yttrium nitrate, 6.51g of cerium nitrate and 1.31g of barium nitrate were dissolved in 100ml of water and stirred to obtain a solution A; processing to obtain final sample Y2Ce1.5Ba0.5O7。
Wherein 6.51g of cerium nitrate and 1.31g of barium nitrate are dissolved in a first dissolving bottle 110 through normal temperature buffering, 7.66g of yttrium nitrate is dissolved in a second dissolving bottle 120 through low temperature buffering, and the solutions in the first dissolving bottle 110 and the second dissolving bottle 120 are mixed in a dissolving beaker on a placing groove through a liquid outlet 13 to obtain a solution A; dissolving barium nitrate, cerium nitrate and yttrium nitrate in sequence, putting the solution in the first dissolving bottle 110 into a dissolving beaker, and putting the solution in the second dissolving bottle 120 into the dissolving beaker.
Test examples
XRD test
XRD analysis was performed on the products prepared at different loadings, as shown in FIG. 1. The results show that: when the amount X of Ba is 0-0.3, the diffraction intensity of the peak continuously increases, the structure of the obtained product is completely consistent with that of the matrix, and no change occurs in the diffraction peak even if the amount X is more than 0.3, so that the effect is best when the amount X is 0.3.
Y at different calcination temperatures when other conditions are the same2Ce2-xBaxO7The XRD pattern of the resulting product is shown in FIG. 2. It can be seen that the product can be successfully synthesized at six temperatures, and the crystallinity of the product becomes better and better with the increase of the temperature, so 900 ℃ is selected as the preferred calcining temperature.
EDS analysis
The product was tested for the area composition by an energy spectrometer, as shown in fig. 4. The figure shows that the doped product is composed of four elements of Y, Ce, Ba and O, the surface distribution is very uniform, and no chemical segregation phenomenon occurs. It is also evident from the figure that: atomic ratio Y: (Ce + Ba) is about 1:1, in stoichiometric terms.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (8)

1. A method for preparing a pyrochlore-structured white inorganic ceramic pigment, wherein the white inorganic ceramic pigment has Y2Ce2-xBaxO7Wherein X is more than or equal to 0.25 and less than or equal to 0.30; the preparation method of the white inorganic ceramic pigment comprises the following steps:
1) respectively dissolving corresponding yttrium nitrate, cerium nitrate and barium nitrate in distilled water on a dissolving device according to the molar ratio of Y, Ce to Ba to obtain a mixed solution;
2) adding the mixed solution obtained in the step 1) into an aqueous solution of glycine;
3) stirring the mixed solution obtained in the step 2) for 1-10 hours at 60 ℃ by using a magnetic stirrer, and then burning and concentrating at 120 ℃ to obtain precursor powder;
4) finally, calcining the precursor powder obtained in the step 3) by using a muffle furnace at the calcining temperature of 500-900 ℃ for 2-4 hours to obtain a white ceramic pigment with a pyrochlore structure; preheating in the early stage before calcination, specifically: putting the precursor powder into a muffle furnace, heating for the first time, heating to 300 ℃ at a heating rate of 5 ℃/min, and then preserving heat for 30-45 min; then adding the mixture into the furnace at a heating rate of 20 ℃/min to 500-900 ℃ for calcination.
2. The method for preparing a pyrochlore-structured white inorganic ceramic pigment according to claim 1, wherein the yttrium nitrate, the cerium nitrate and the barium nitrate in step 1) are dissolved in the distilled water in the order of dissolving the barium nitrate, dissolving the cerium nitrate and dissolving the yttrium nitrate.
3. The method for preparing a pyrochlore-structured white inorganic ceramic pigment according to claim 1 wherein the agitation in step 3) is at a rate of from 80 to 100 r/min.
4. The method for preparing a pyrochlore-structured white inorganic ceramic pigment according to claim 1, wherein the mixed solution in step 3) is stirred for 1.5 to 2 hours.
5. The method for preparing a pyrochlore-structured white inorganic ceramic pigment according to claim 1 wherein the calcination temperature in step 4) is 900 ℃.
6. The method for preparing a pyrochlore-structured white inorganic ceramic pigment according to claim 1, wherein the calcination time in step 4) is 3 to 4 hours.
7. The method for preparing a pyrochlore-structured white inorganic ceramic pigment according to claim 1, wherein the dissolving device in step 1) comprises a base, a buffer tank (1), a vibrating device (2) and a condensing device (3), wherein the buffer tank (1) is arranged on the base through a support rod, and the vibrating device (2) is arranged on the base and is positioned below the buffer tank (1); the buffer tank (1) comprises a normal-temperature dissolution cavity (11) and a low-temperature dissolution cavity (12), a liquid outlet (13) is formed in the lower end of the buffer tank (1), a first dissolution bottle (110) is arranged inside the normal-temperature dissolution cavity (11), a second dissolution bottle (120) is arranged inside the low-temperature dissolution cavity (12), the condensing device (3) is arranged in the low-temperature dissolution cavity (12) and located below the second dissolution bottle (120), the first dissolution bottle (110) and the second dissolution bottle (120) are respectively connected with the liquid outlet (13) through connecting pipes, and a first valve and a second valve are respectively arranged at the joints; the outer side walls of the normal-temperature dissolving cavity (11) and the low-temperature dissolving cavity (12) are provided with a first valve switch (111) and a second valve switch (121) which correspond to the first valve and the second valve, and the side wall of the buffer tank (1) is provided with a control panel (31) of the condensing device (3); the oscillating device (2) comprises an oscillating motor (21), a swing connecting rod (22) and a clamping seat (23), wherein the oscillating motor (21) provides power for the swing connecting rod (22), the clamping seat (23) is arranged at the upper end of the swing connecting rod (22), a placing groove is formed in the clamping seat (23), the placing groove is located under the liquid outlet (13), and the placing groove is used for placing a dissolving beaker.
8. A method for preparing a pyrochlore structure white inorganic ceramic pigment as claimed in claim 7 wherein the condensing means (3) is set at a temperature of from 2 ℃ to 5 ℃.
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