CN116769330A - Preparation method of praseodymium-zirconium yellow ceramic pigment with glaze reinforcing and toughening effects - Google Patents
Preparation method of praseodymium-zirconium yellow ceramic pigment with glaze reinforcing and toughening effects Download PDFInfo
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- CN116769330A CN116769330A CN202310796147.5A CN202310796147A CN116769330A CN 116769330 A CN116769330 A CN 116769330A CN 202310796147 A CN202310796147 A CN 202310796147A CN 116769330 A CN116769330 A CN 116769330A
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- 239000000049 pigment Substances 0.000 title claims abstract description 38
- 239000000919 ceramic Substances 0.000 title claims abstract description 35
- USEGQPUGEPSVQL-UHFFFAOYSA-N [Pr].[Zr] Chemical compound [Pr].[Zr] USEGQPUGEPSVQL-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 230000000694 effects Effects 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 230000003014 reinforcing effect Effects 0.000 title claims description 6
- 238000000227 grinding Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 10
- 229910052726 zirconium Inorganic materials 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003086 colorant Substances 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- SNMVRZFUUCLYTO-UHFFFAOYSA-N n-propyl chloride Chemical compound CCCCl SNMVRZFUUCLYTO-UHFFFAOYSA-N 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 150000004689 octahydrates Chemical class 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 150000003376 silicon Chemical class 0.000 claims description 2
- UVGLBOPDEUYYCS-UHFFFAOYSA-N silicon zirconium Chemical compound [Si].[Zr] UVGLBOPDEUYYCS-UHFFFAOYSA-N 0.000 claims description 2
- 150000003754 zirconium Chemical class 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 4
- 230000002787 reinforcement Effects 0.000 abstract description 3
- 238000009877 rendering Methods 0.000 abstract description 2
- 238000005728 strengthening Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000001052 yellow pigment Substances 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 2
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910006501 ZrSiO Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- HZGFMPXURINDAW-UHFFFAOYSA-N iron zirconium Chemical compound [Fe].[Zr].[Zr] HZGFMPXURINDAW-UHFFFAOYSA-N 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000012720 thermal barrier coating Substances 0.000 description 1
- PSUYMGPLEJLSPA-UHFFFAOYSA-N vanadium zirconium Chemical compound [V].[V].[Zr] PSUYMGPLEJLSPA-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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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
- C09C1/0009—Pigments for ceramics
- C09C1/0012—Pigments for ceramics containing zirconium and silicon
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
- C01P2006/62—L* (lightness axis)
-
- 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
- C01P2006/63—Optical properties, e.g. expressed in CIELAB-values a* (red-green axis)
-
- 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
- C01P2006/64—Optical properties, e.g. expressed in CIELAB-values b* (yellow-blue axis)
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a preparation method of praseodymium-zirconium yellow ceramic pigment with glaze strengthening and toughening effects, which improves the chemical activity of a reaction precursor by means of simple mechanical grinding, increases the dispersibility of the precursor by introducing a grinding aid in the grinding process, then carries out heat treatment on a uniformly mixed grinding product at a specified temperature, and repeatedly washes and dries to obtain whisker-shaped praseodymium-zirconium yellow ceramic pigment powder with good dispersibility and excellent color rendering performance. The invention has low raw material cost, simple process and short preparation period, and is suitable for mass production of products. The prepared whisker-shaped praseodymium-zirconium yellow ceramic pigment has good dispersibility and uniform size, can play a role in whisker reinforcement and toughening when being used as a pigment, and effectively improves the glaze strength and toughness.
Description
Technical Field
The invention belongs to the field of inorganic nonmetallic materials, and particularly relates to a preparation method of praseodymium-zirconium yellow ceramic pigment with a glaze reinforcing and toughening effect.
Background
Zirconium silicate has the excellent characteristics of high melting point (2500 ℃), high strength, oxidation resistance, excellent thermal shock resistance, wear resistance, melt erosion resistance and the like, and is widely applied to the fields of refractory materials, thermal barrier coatings, nuclear waste storage, high-temperature ceramic pigment matrixes, reinforcement and toughening and the like. In the field of high-temperature ceramic pigments, zirconium silicate-based ceramic pigments occupy an important role, particularly zirconium-based three primary colors, including vanadium-zirconium blue, praseodymium-zirconium yellow and iron-zirconium red, are the only ceramic pigments capable of generating three colors with the same matrix at present, and therefore have good miscibility. Among them, praseodymium zirconium yellow is attracting attention in its vivid and noble yellow tone, and can make the glaze exhibit vivid yellow tone and stable color.
The existing preparation method of praseodymium-zirconium yellow ceramic pigment mainly comprises two main categories: one type is a solid phase method, and the other type is a liquid phase method. The traditional solid phase method uses oxide as a precursor, the activity is lower, the particle size of the prepared pigment particles is large and the size is uneven, the pigment particles are difficult to uniformly mix with glaze, and further ball milling treatment is needed. The micro morphology of the pigment powder prepared by the liquid phase method is mostly agglomerate or irregularly shaped small particles [ Wang Y, lai F, wang Q, et al Synthesis and chromatic properties of high color performance Pr ] x -ZrSiO 4 (x=0-0.1) yellow pigment[J].Journal of Alloys and Compounds, 2022(891):161932-161942.]The reinforcing and toughening effects are limited, and the color cast problem of the pigment is easily caused. The reason is that the precursor selected by the method has poor activity or dispersibility, so that the morphology of the finally grown pigment particles is irregular or the agglomeration is serious. In comparison, whiskers have been widely used in the field of reinforcement and toughening, and the toughness and strength of a base material can be remarkably increased by utilizing the bridging effect and the pulling-out effect of the whiskers. Ceramic products, particularly daily porcelain, often need to face abrasion, rubbing and high-pressure flushing and other tests in the use process, so that higher requirements on the abrasion resistance, strength, toughness and the like of the glaze are provided. Therefore, if a whisker-like praseodymium-zirconium yellow ceramic coloring material can be prepared, it can not only exert the zirconium silicateThe wear-resistant and corrosion-resistant properties of the glaze can be utilized to effectively strengthen and toughen the glaze while the bright yellow color is maintained, and the service life of the glaze is greatly prolonged.
Disclosure of Invention
The invention aims to solve the technical problem of providing the praseodymium-zirconium yellow ceramic pigment with low raw material cost, simple process, short preparation period and glaze strengthening and toughening effects, which is suitable for industrial production.
In order to solve the technical problems, the technical scheme of the invention is as follows: the preparation method of the praseodymium-zirconium yellow ceramic pigment with the glaze reinforcing and toughening effects is characterized by comprising the following steps of:
step one: weighing silicon salt and zirconium salt with corresponding mass according to a certain silicon-zirconium molar ratio, weighing mineralizer and colorant with a certain proportion, and uniformly mixing the raw materials to obtain a mixed product;
step two: adding a certain volume of grinding aid into the mixed product, and mechanically grinding for 15 minutes to obtain a praseodymium-zirconium yellow ceramic pigment precursor mixture;
step three: carrying out heat treatment on the praseodymium-zirconium yellow ceramic pigment precursor mixture at a set temperature, and naturally cooling the mixture along with a furnace to obtain a calcined product;
step four: and repeatedly cleaning the obtained calcined product by deionized water, and drying at 70 ℃ to obtain the whisker-shaped praseodymium-zirconium yellow ceramic pigment.
The silicon source in the step one is Na 2 SiO 3 ·9H 2 The O, zirconium source is ZrOCl octahydrate 2 ·8H 2 O。
In the first step, the molar ratio of the silicon source to the zirconium source is 1-1.15.
In the first step, the mineralizer is LiF or NaF, and the dosage of the mineralizer is F/Zr mole ratio of 0.2-0.5.
The colorant in the first step is PrCl 3 ·6H 2 O, the dosage of which is Pr/Zr mole ratio 0.03-0.07.
In the second step, the grinding aid is one of ethanol, glycol and isopropanol, and the added volume of the grinding aid is 3-5 mL corresponding to each 10mmol of zirconium source.
The heat treatment system in the third step is that the calcination temperature is 850-950 ℃ and the heat preservation time is 3-7 h.
The invention adopts the soft mechanochemical assistance to prepare the whisker praseodymium-zirconium yellow ceramic pigment powder. The soft mechanochemical treatment can improve the activity of the precursor and simultaneously reduce the agglomeration of the precursor by adding the grinding aid, and finally, the high-dispersion whisker-shaped sample is obtained by further heat treatment and water washing. The obtained praseodymium-zirconium yellow pigment powder has excellent color rendering performance, and the high-dispersion whisker structure can effectively increase the strength and toughness of the glaze, so that the praseodymium-zirconium yellow pigment powder has important application value.
Drawings
FIG. 1 is an XRD pattern of a whisker-like praseodymium-zirconium yellow ceramic pigment of example 1;
FIG. 2 is an SEM photograph of a whisker-like praseodymium-zirconium yellow ceramic coloring material of example 1.
Detailed Description
The invention will be described in further detail with reference to the drawings and the detailed description.
Example 1
Weigh 3.2225 g ZrOCl 2 ·8H 2 O（10 mmol），2.8422 g Na 2 SiO 3 ·9H 2 O (10 mmol), liF (2 mmol) of 0.0519 g, prCl of 0.1777 g 3 ·6H 2 O (0.5 mmol), wherein the molar ratio of the silicon source to the zirconium source is 1, the molar ratio of F/Zr is 0.2, the molar ratio of Pr/Zr is 0.05, the raw materials are uniformly mixed in an agate mortar, 3mL of absolute ethyl alcohol is added, mechanical grinding is continued for 15 min to obtain a precursor mixture, then the precursor mixture is heated to 900 ℃ and kept for 5h, natural cooling is carried out, deionized water is used for repeatedly washing and drying is carried out at 70 ℃, and whisker-shaped praseodymium-zirconium yellow ceramic pigment powder is obtained, and the chroma L, the a and the b of the test powder are 84.46, -4.82 and 50.75 respectively.
Example 2
Na in example 1 2 SiO 3 ·9H 2 The addition amount of O is changed to 3.2685 g (11.5 mmol), the addition amount of LiF is changed to 0.1298 g (5 mmol), the corresponding mole ratio of silicon source to zirconium source is 1.15, the mole ratio of F/Zr is 0.5, the heat treatment system is changed to 850 ℃ and the temperature is kept at 7 h, other stripsThe product is unchanged, and the whisker-shaped praseodymium-zirconium yellow ceramic pigment powder is finally obtained.
Example 3
PrCl in example 1 3 ·6H 2 The addition amount of O is changed to 0.1066 (0.3 mmol), the corresponding Pr/Zr molar ratio is 0.03, the mineralizer is changed to 0.0840 g NaF (2 mmol), the grinding aid is changed to 4mL glycol, the heat treatment system is changed to 950, and the temperature is kept at 3 h, so that the whisker-shaped praseodymium-zirconium yellow ceramic pigment powder is finally obtained.
Example 4
The LiF addition in example 1 was changed to 0.1038 g (4 mmol), prCl 3 ·6H 2 The addition amount of O is changed to 0.2488 (0.7 mmol), the corresponding F/Zr molar ratio is 0.4, the Pr/Zr molar ratio is 0.07, the grinding aid is changed to 5mL of isopropanol, and other conditions are unchanged, so that the whisker-shaped praseodymium-zirconium yellow ceramic pigment powder is finally obtained.
The above-described embodiments are merely illustrative of the principles and functions of the present invention, and some of the practical examples, not intended to limit the invention; it should be noted that modifications and improvements can be made by those skilled in the art without departing from the inventive concept, and these are all within the scope of the present invention.
Claims (7)
1. The preparation method of the praseodymium-zirconium yellow ceramic pigment with the glaze reinforcing and toughening effects is characterized by comprising the following steps of:
step one: weighing silicon salt and zirconium salt with corresponding mass according to a certain silicon-zirconium molar ratio, weighing mineralizer and colorant with a certain proportion, and uniformly mixing the raw materials to obtain a mixed product;
step two: adding a certain volume of grinding aid into the mixed product, and mechanically grinding for 15 minutes to obtain a praseodymium-zirconium yellow ceramic pigment precursor mixture;
step three: carrying out heat treatment on the praseodymium-zirconium yellow ceramic pigment precursor mixture at a set temperature, and naturally cooling the mixture along with a furnace to obtain a calcined product;
step four: and repeatedly cleaning the obtained calcined product by deionized water, and drying at 70 ℃ to obtain the whisker-shaped praseodymium-zirconium yellow ceramic pigment.
2. The method for preparing the praseodymium-zirconium yellow ceramic pigment according to claim 1, which is characterized in that: the silicon source in the step one is Na 2 SiO 3 ·9H 2 The O, zirconium source is ZrOCl octahydrate 2 ·8H 2 O。
3. The method for preparing the praseodymium-zirconium yellow ceramic pigment according to claim 1, which is characterized in that: in the first step, the molar ratio of the silicon source to the zirconium source is 1-1.15.
4. The method for preparing the praseodymium-zirconium yellow ceramic pigment according to claim 1, which is characterized in that: in the first step, the mineralizer is LiF or NaF, and the dosage of the mineralizer is F/Zr mole ratio of 0.2-0.5.
5. The method for preparing the praseodymium-zirconium yellow ceramic pigment according to claim 1, which is characterized in that: the colorant in the first step is PrCl 3 ·6H 2 O, the dosage of which is Pr/Zr mole ratio 0.03-0.07.
6. The method for preparing the praseodymium-zirconium yellow ceramic pigment according to claim 1, which is characterized in that: in the second step, the grinding aid is one of ethanol, glycol and isopropanol, and the added volume of the grinding aid is 3-5 mL corresponding to each 10mmol of zirconium source.
7. The method for preparing the praseodymium-zirconium yellow ceramic pigment according to claim 1, which is characterized in that: the heat treatment system in the third step is that the calcination temperature is 850-950 ℃ and the heat preservation time is 3-7 h.
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| CN202310796147.5A CN116769330A (en) | 2023-07-01 | 2023-07-01 | Preparation method of praseodymium-zirconium yellow ceramic pigment with glaze reinforcing and toughening effects |
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| CN202310796147.5A CN116769330A (en) | 2023-07-01 | 2023-07-01 | Preparation method of praseodymium-zirconium yellow ceramic pigment with glaze reinforcing and toughening effects |
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