CN105130499A - Compound type ultrafine yellow ceramic pigment and preparation method thereof - Google Patents
Compound type ultrafine yellow ceramic pigment and preparation method thereof Download PDFInfo
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- CN105130499A CN105130499A CN201510511420.0A CN201510511420A CN105130499A CN 105130499 A CN105130499 A CN 105130499A CN 201510511420 A CN201510511420 A CN 201510511420A CN 105130499 A CN105130499 A CN 105130499A
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Abstract
The invention belongs to the technical field of ceramic pigments, and concretely relates to a compound type ultrafine yellow ceramic pigment and a preparation method thereof. The preparation method concretely comprises 1) dissolving nickel titanate in water to obtain a solution A; 2) uniformly mixing butyl titanate and anhydrous ethanol being 2-3 times by volume of butyl titanate, so as to obtain a solution B; 3) adding the solution B into the solution A under the stirring condition, stirring at room temperature for 5 h or more, and then standing for ageing for 24-48 h, so as to obtain an opaque gel; and 4) drying and grinding the opaque gel obtained in the step 3) to obtain a loosen precursor powder, then transferring into a muffle furnace, and roasting at 400-500 DEG C for 4-6 h, so as to obtain the yellow ceramic pigment. The compound type ultrafine yellow ceramic pigment obtained through the preparation method combines excellent performances of NiTiO3 and TiO2, and possesses advantages of bright color, no color variation at high temperature, and the like.
Description
Technical field
The invention belongs to beramic color technical field, be specifically related to a kind of compound ultra-fine yellow beramic color and preparation method thereof.
Background technology
The yellow monochromatic color that should be wavelength 597-577nm in meaning physically, no matter yellow beramic color is for ceramic illuminated, or is all the indispensable finishing material of ceramic decoration art as the toner of ceramic colour glaze or look embryo.Traditional yellow ultramarine comprises poisonous heavy metal mostly as lead, chromium etc., cause serious impact, and the pigment of traditional single performance can not meet the demand of all trades and professions on environment and individual.We know, after scantling drops to nano level, just to have the unrivaled high-performance of conventional material simultaneously.Therefore, seek green synthetic method, in relatively gentle environment, obtain that size is little, the high-performance nano yellow ultramarine of good dispersity, even particle size distribution is imperative.
Conventional TiO
2be the heat insulation pigment of a kind of high infrared reflection, it is fluffy white powder, and shielding ultraviolet rays effect is strong, has good dispersiveness and weathering resistance.But because its self outward appearance is white, so be easy to cause white pollution, pollution to a certain degree caused to air, has also injured the retina of people to a certain extent.
Application number is the preparation method that application discloses a kind of inorganic-organic hybrid yellow ultramarine of 201410405705.1, although this pigment has the advantage such as Heat stability is good, good light stability, and this compound yellow ultramarine is compared with Inorganic yellow pigment lead-chrome yellow, show more excellent tinctorial property, as tinting strength is higher, color is more bright-coloured, yellow is more pure, but the complex operation step in its preparation process, scale operation is difficult to ensure the quality of products, and cost is higher; And synthesis temperature is high, be unfavorable for suitability for industrialized production.
Summary of the invention
The object of the invention is to overcome prior art defect, and provide compound ultra-fine yellow beramic color of a kind of inorganic-inorganic and preparation method thereof, it is by active TiO
2with yellow ultramarine NiTiO
3carry out compound, synthesize the Yellow environment-friendly mineral dye of high brightness at a lower temperature.
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for compound ultra-fine yellow beramic color, it comprises the steps:
1) nickel titanate is soluble in water, obtain solution A;
2) butyl (tetra) titanate is mixed with 2-3 volume dehydrated alcohol doubly, obtain solution B; The butyl (tetra) titanate added is in titanium dioxide, and the addition of nickel titanate is 2-10 times of titanium dioxide quality;
3) under agitation solution B is dropwise joined in solution A, more than stirring at room temperature 5h, more still aging 24-48h obtains opaque gel;
4) the opaque gel drying of step 3) gained, grinding obtain loose precursor powder, then to proceed in retort furnace in 400-500 DEG C of roasting 4-6h, obtain yellow beramic color.
Concrete, the stirring velocity in step 3) is preferably 80-100 rev/min; Drying conditions in step 4) is preferably: 80 DEG C of dry 4h of elder generation, then 90 DEG C of dry 2h.
Nickel titanate (NiTiO described in step 1)
3) obtain through following method: by Ni (NO
3)
26H
2o and butyl (tetra) titanate join in the aqueous solution of glycine, first stir to clarify at 60 ± 10 DEG C and be then heated to 100-120 DEG C of stirring 100 ± 10min, the reaction of solution generation self-propagating combustion generates loose powder in the process, and gained powder is calcined in 700-900 DEG C and be get final product.
In the preparation process of above-mentioned nickel titanate, the Ni (NO of interpolation
3)
26H
2o, butyl (tetra) titanate are respectively in Ni, Ti, and glycine molar weight is 2 times of Ni, Ti molar weight sum; Calcining temperature is preferably 750-850 DEG C, further preferred 800-850 DEG C.
The compound ultra-fine yellow beramic color adopting above-mentioned either method to prepare.
In the preparation process of nickel titanate, calcining temperature is when 700-900 DEG C, and gained nickel titanate is dispersed general, and colour generation is general; Calcining temperature is when 750-850 DEG C, and gained nickel titanate is better dispersed, and colour generation is better; Calcining temperature is when 800-850 DEG C, and gained nickel titanate dispersiveness is best, and colour generation is also best.
Stirring at room temperature time preferred 5-6h in step 3).The stirring reaction time is less than 5h, and product fully can not react compound, causes product mutually uneven.In step 4), maturing temperature is when 400-500 DEG C, and the compound ultra-fine yellow beramic color product of gained is better dispersed, and size-grade distribution is more even.If calcining temperature too low (being less than 400 DEG C), then product can not abundant compound, shows as color impure; If calcining temperature too high (being greater than 500 DEG C), although the colourity of product is without considerable change, suitability for industrialized production power consumption will increase greatly.
Compared to the prior art, beneficial effect of the present invention:
The present invention is by NiTiO
3yellow ultramarine and TiO
2compound, by the synergistic effect of the two, performs to the best by the advantage of the two, has synthesized NiTiO
3/ TiO
2nano composite ceramic pigment.The compound ultra-fine yellow beramic color of gained of the present invention combines NiTiO
3and TiO
2premium properties, there is the advantage such as lovely luster, high temperature nondiscoloration.In addition, preparation method of the present invention is simple, and raw material is easy to get, and synthesis temperature is low, and technique is simply controlled, is suitable for large-scale production; And products obtained therefrom is low molecule, low toxicity even non-toxic organic thing, the not toxic element such as leaded chromium, environmental protection, product particles good dispersity, even particle size distribution, colour generation is good.
Accompanying drawing explanation
Fig. 1 is NiTiO
3x-ray diffraction spectrogram before and after compound;
Fig. 2 is TiO
2measure identical, under different maturing temperature (400,500 DEG C), the compound (NiTiO of embodiment 2 and 4
3/ TiO
2) the X-ray diffraction spectrogram of ultra-fine yellow beramic color;
Fig. 3 is the NiTiO under different calcining temperature, identical magnification
3sEM photo; In figure, a calcining temperature is 700 DEG C, and b calcining temperature is 800 DEG C, and c calcining temperature is 900 DEG C;
Fig. 4 is the NiTiO of same magnification
3sEM photo before and after compound;
Fig. 5 is NiTiO
3the partial face scanning of compound after product can spectrogram.
Fig. 6 is NiTiO
3the energy spectrum analysis figure of compound after product.
Embodiment
Do to introduce in detail further to technical scheme of the present invention below in conjunction with embodiment, but protection scope of the present invention is not limited thereto.
niTiO
3
preparation example 1
First 30g glycine is dissolved in 100mL distilled water, then adds the Ni (NO of 29.1g
3)
26H
2the butyl (tetra) titanate of O and 34g, being placed on design temperature is stirring and dissolving on the magnetic stirring apparatus of 60 DEG C, obtains clear liquor (about needing 20min) completely to dissolving.Then be heated to 110 DEG C of reaction 100min, liquid thickness expands, and then discharges gas in the process, self-propagating combustion reaction occurs rapidly, generates loose powder.Gained powder calcines 4h at 700 DEG C, i.e. Yellow nanometer pigment NiTiO
3.
niTiO
3
preparation example 2
First 30g glycine is dissolved in 100mL distilled water, then adds the Ni (NO of 29.1g successively
3)
26H
2the butyl (tetra) titanate of O and 34g, being placed on design temperature is the magnetic stirring apparatus of 60 DEG C dissolves stir, and obtains clear liquor (about needing 20min) completely to dissolving.Then 110 DEG C of reaction 100min are heated to, liquid thickness expansion in the process, ' discharge gas, there is rapidly self-propagating combustion reaction, generate the powder loosened.Gained powder calcines 4h at 800 DEG C, obtains Yellow nanometer pigment NiTiO
3.
niTiO
3
preparation example 3
First 30g glycine is dissolved in during 120mL distilled water goes, then adds the Ni (NO of 29.1g successively
3)
26H
2the butyl (tetra) titanate of O and 34g, being placed on design temperature is the magnetic stirring apparatus of 60 DEG C dissolves stir, and obtains clear liquor (about needing 20min) completely to dissolving.Then be heated to 110 DEG C of reaction 100min, liquid thickness expands, and then discharges gas in the process, self-propagating combustion reaction occurs rapidly, generates loose powder.Gained powder calcines 4h at 900 DEG C, obtains Yellow nanometer pigment NiTiO
3.
By the NiTiO of preparation example 2 gained
3for the preparation of following compound ultra-fine yellow beramic color.
embodiment 1
A preparation method for compound ultra-fine yellow beramic color, it comprises the steps:
1) 2g nickel titanate is joined in 100mL water, stir, obtain solution A;
2) 0.852g butyl (tetra) titanate (being 0.2g titanium dioxide after converting) is mixed with 3 volumes dehydrated alcohol doubly, obtain solution B;
3) solution B dropwise joined in solution A under agitation, with stirring at room temperature 6h under the speed of 90 revs/min, more still aging 48h obtains opaque gel;
4) the opaque gel of step 3) gained is at 80 DEG C of dry 4h of elder generation, then 90 DEG C of dry 2h, then obtains loose precursor powder through grinding, finally to proceed in retort furnace in 400 DEG C of roasting 5h, obtains compound (NiTiO
3/ TiO
2) ultra-fine yellow beramic color.
embodiment 2
A preparation method for compound ultra-fine yellow beramic color, it comprises the steps:
1) 2g nickel titanate is joined in 100mL water, stir, obtain solution A;
2) 3.409g butyl (tetra) titanate (being 0.8g titanium dioxide after converting) is mixed with 2 volumes dehydrated alcohol doubly, obtain solution B;
3) solution B dropwise joined in solution A under agitation, with stirring at room temperature 5h under the speed of 90 revs/min, more still aging 24h obtains opaque gel;
4) the opaque gel of step 3) gained is at 80 DEG C of dry 4h of elder generation, then 90 DEG C of dry 2h, then obtains loose precursor powder through grinding, finally to proceed in retort furnace in 400 DEG C of roasting 5h, obtains compound (NiTiO
3/ TiO
2) ultra-fine yellow beramic color.
embodiment 3
A preparation method for compound ultra-fine yellow beramic color, it comprises the steps:
1) 2g nickel titanate is joined in 100mL water, stir, obtain solution A;
2) 0.852g butyl (tetra) titanate (being 0.2g titanium dioxide after converting) is mixed with 3 volumes dehydrated alcohol doubly, obtain solution B;
3) solution B dropwise joined in solution A under agitation, with stirring at room temperature 6h under the speed of 100 revs/min, more still aging 48h obtains opaque gel;
4) the opaque gel of step 3) gained is at 80 DEG C of dry 4h of elder generation, then 90 DEG C of dry 2h, then obtains loose precursor powder through grinding, finally to proceed in retort furnace in 500 DEG C of roasting 5h, obtains compound (NiTiO
3/ TiO
2) ultra-fine yellow beramic color.
embodiment 4
A preparation method for compound ultra-fine yellow beramic color, it comprises the steps:
1) 2g nickel titanate is joined in 100mL water, stir, obtain solution A;
2) 3.409g butyl (tetra) titanate (being 0.8g titanium dioxide after converting) is mixed with 2 volumes dehydrated alcohol doubly, obtain solution B;
3) solution B dropwise joined in solution A under agitation, with stirring at room temperature 5h under the speed of 90 revs/min, more still aging 24h obtains opaque gel;
4) the opaque gel of step 3) gained is at 80 DEG C of dry 4h of elder generation, then 90 DEG C of dry 2h, then obtains loose precursor powder through grinding, finally to proceed in retort furnace in 500 DEG C of roasting 5h, obtains compound (NiTiO
3/ TiO
2) ultra-fine yellow beramic color.
xRD tests
To pure NiTiO
3(NiTiO compound with the present invention
3/ TiO
2) ultra-fine yellow beramic color carried out XRD analysis, as shown in Figure 1.Result is known: with pure NiTiO
3compare, the compound (NiTiO of the present invention
3/ TiO
2) TiO appearred in ultra-fine yellow beramic color
2characteristic diffraction peak, consistent with the set goal.
Identical TiO
2amount, the compound (NiTiO of different maturing temperature
3/ TiO
2) the XRD figure type of ultra-fine yellow beramic color, as shown in Figure 2.Result is known: after 400 DEG C of roasting 5h, has occurred TiO
2characteristic diffraction peak, continue ascending temperature be after 500 DEG C, there is stronger TiO
2characteristic diffraction peak, consider based on energy conservation, preferred maturing temperature is 400 DEG C.
sEM tests
Carry out micro-structural test by scanning electron microscope to product, Fig. 3 is the NiTiO under different calcining temperature, identical magnification
3sEM photo.From photo, we can clearly find out: matrix NiTiO3 has good dispersiveness, and size distribution is more even.Meanwhile, can observe when temperature is from 700 DEG C to 900 DEG C, the mean sizes of crystal grain constantly increases, size at about 50nm, in nano level scope, so this material belongs to nano material category.Fig. 4 is the NiTiO of same magnification
3sEM photo before and after compound, this photo illustrates combination product (NiTiO
3/ TiO
2) pattern become spherical from particulate state, surface because of coated TiO
2and seem that some is coarse.Compound NiTiO
3/ TiO
2the good dispersity of material, even particle size distribution.For pigment, granularity is less, and particle specific surface is larger, and specific surface energy is higher, and material scatter is good in addition, in use easily forms uniform coating, and strong adhesion, evenness.
eDS tests
Carried out face moiety test by energy spectrometer to product, as illustrated in Figures 5 and 6, Fig. 5 is NiTiO
3/ TiO
2the Surface scan energy spectrogram of nano material, this figure illustrates the product NiTiO after compound
3/ TiO
2to be made up of element Ni, Ti, O tri-kinds of elements and surface arrangement is very even, not occur chemical segregation phenomena.Fig. 6 is NiTiO
3/ TiO
2energy spectrum analysis figure before and after compound, through contrast, we can clearly find out: NiTiO
3after compound, the content of element Ni obviously reduces, and the content of element ti increases greatly.This explanation can make activating oxide TiO in this way
2be coated on NiTiO
3on the surface.In addition, the atomic ratio of Ni/Ti is less than 1:1.This is because after compound, NiTiO
3nanocrystalline coated by TiO2 institute, element Ni is wrapped in inside nano material, so content reduces, and element ti is attached to particle surface, adds NiTiO
3the Ti element self comprised, so atom content can increase.
colourity is tested
Prepared by embodiment 1 and 2 to the compound (NiTiO of gained
3/ TiO
2) ultra-fine yellow beramic color carries out colourity test, the results are shown in Table 1.
Table 1 is NiTiO
3with TiO
2the color coordinates schematic diagram of combination product
As can be seen from Table 1: along with activating oxide TiO
2the increase of amount, the value of a* is in a slight decrease, and b* is increased to 38.7 from 21.2 of matrix.And lightness L* is in continuous increase, increase to 51.0 by 42.3.Illustrate within the specific limits, along with TiO
2the increase of content, the color of combination product is more tending towards glassy yellow.Wherein, L* is brightness; A* is red green changing value, and a* larger expression product colour is redder; B* is yellowish green changing value, and b* larger expression product colour is more yellow.
mechanism of the present invention is as follows:
NiTiO
3matrix is the perovskite structure that a class has extensive chemical stability, water insoluble, is insoluble to ethanol, is insoluble to acid.And TiO
2be the heat insulation pigment of a kind of high infrared reflection, but shortcoming is the white appearance due to it, is easy to cause " white light " to pollute, the retina of harm people.Therefore, the two effectively combined, energy compound goes out the high infrared reflection insulating color pigment of high comprehensive performance.
Claims (7)
1. a preparation method for compound ultra-fine yellow beramic color, is characterized in that, comprise the steps:
1) nickel titanate is soluble in water, obtain solution A;
2) butyl (tetra) titanate is mixed with 2-3 volume dehydrated alcohol doubly, obtain solution B; The butyl (tetra) titanate added is in titanium dioxide, and the addition of nickel titanate is 2-10 times of titanium dioxide quality;
3) under agitation solution B is joined in solution A, more than stirring at room temperature 5h, more still aging 24-48h obtain opaque gel;
4) the opaque gel drying of step 3) gained, grinding obtain loose precursor powder, then to proceed in retort furnace in 400-500 DEG C of roasting 4-6h, obtain yellow beramic color.
2. the preparation method of compound ultra-fine yellow beramic color as claimed in claim 1, it is characterized in that, the stirring velocity in step 3) is 80-100 rev/min; Drying conditions in step 4) is specially: 80 DEG C of dry 4h of elder generation, then 90 DEG C of dry 2h.
3. the preparation method of compound ultra-fine yellow beramic color as claimed in claim 1, it is characterized in that, the nickel titanate described in step 1) obtains through following method: by Ni (NO
3)
26H
2o and butyl (tetra) titanate join in the aqueous solution of glycine, first stir to clarify at 60 ± 10 DEG C, then be heated to 100-120 DEG C and stir 100 ± 10min, the reaction of solution generation self-propagating combustion generates loose powder in the process, and gained powder is calcined in 700-900 DEG C and be get final product.
4. the preparation method of compound ultra-fine yellow beramic color as claimed in claim 3, is characterized in that, the Ni (NO of interpolation
3)
26H
2o, butyl (tetra) titanate are respectively in Ni, Ti, and glycine molar weight is 2 times of Ni, Ti molar weight sum.
5. the preparation method of compound ultra-fine yellow beramic color as claimed in claim 3, it is characterized in that, calcining temperature is 750-850 DEG C.
6. the preparation method of compound ultra-fine yellow beramic color as claimed in claim 5, it is characterized in that, calcining temperature is 800-850 DEG C.
7. adopt the compound ultra-fine yellow beramic color that the arbitrary described method of claim 1 to 6 prepares.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107987559A (en) * | 2017-12-05 | 2018-05-04 | 华北水利水电大学 | A kind of spherical compound superfine red ceramic paint and preparation method thereof |
| CN107987558A (en) * | 2017-12-05 | 2018-05-04 | 华北水利水电大学 | A kind of flowers shape LaFexEu1-xO3/TiO2The preparation method of compound superfine red ceramic paint |
| CN108017936A (en) * | 2017-12-05 | 2018-05-11 | 华北水利水电大学 | A kind of preparation method of spherical compound ultra-fine yellow ceramic paint |
| CN108383385A (en) * | 2018-05-10 | 2018-08-10 | 天长市天意玻璃制品有限公司 | A kind of preparation method of harmless yellow ceramic glaze |
| CN108929569A (en) * | 2018-08-24 | 2018-12-04 | 华北水利水电大学 | A kind of compound red ceramic color LaFeO3/Si02Preparation method |
| CN111205674B (en) * | 2020-01-20 | 2021-11-09 | 大连交通大学 | Ceramic pigment composition, yellow glass ceramic pigment, glass ceramic and preparation method thereof |
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| US20050196605A1 (en) * | 2004-03-08 | 2005-09-08 | Ecology Coatings, Inc. | Environmentally friendly coating compositions for coating metal objects, coated objects therefrom, and methods, processes and assemblages for coating thereof |
| CN104230378A (en) * | 2014-08-29 | 2014-12-24 | 华北水利水电大学 | Perovskite-type superfine yellow ceramic pigment and preparation method thereof |
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2015
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050196605A1 (en) * | 2004-03-08 | 2005-09-08 | Ecology Coatings, Inc. | Environmentally friendly coating compositions for coating metal objects, coated objects therefrom, and methods, processes and assemblages for coating thereof |
| CN104230378A (en) * | 2014-08-29 | 2014-12-24 | 华北水利水电大学 | Perovskite-type superfine yellow ceramic pigment and preparation method thereof |
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|---|---|---|---|---|
| CN107987559A (en) * | 2017-12-05 | 2018-05-04 | 华北水利水电大学 | A kind of spherical compound superfine red ceramic paint and preparation method thereof |
| CN107987558A (en) * | 2017-12-05 | 2018-05-04 | 华北水利水电大学 | A kind of flowers shape LaFexEu1-xO3/TiO2The preparation method of compound superfine red ceramic paint |
| CN108017936A (en) * | 2017-12-05 | 2018-05-11 | 华北水利水电大学 | A kind of preparation method of spherical compound ultra-fine yellow ceramic paint |
| CN107987558B (en) * | 2017-12-05 | 2020-03-31 | 华北水利水电大学 | Flower cluster-shaped LaFexEu1-xO3/TiO2Preparation method of composite superfine red ceramic pigment |
| CN107987559B (en) * | 2017-12-05 | 2020-04-07 | 华北水利水电大学 | Spherical composite superfine red ceramic pigment and preparation method thereof |
| CN108383385A (en) * | 2018-05-10 | 2018-08-10 | 天长市天意玻璃制品有限公司 | A kind of preparation method of harmless yellow ceramic glaze |
| CN108383385B (en) * | 2018-05-10 | 2021-05-07 | 天长市天意玻璃制品有限公司 | Preparation method of harmless yellow ceramic glaze |
| CN108929569A (en) * | 2018-08-24 | 2018-12-04 | 华北水利水电大学 | A kind of compound red ceramic color LaFeO3/Si02Preparation method |
| CN111205674B (en) * | 2020-01-20 | 2021-11-09 | 大连交通大学 | Ceramic pigment composition, yellow glass ceramic pigment, glass ceramic and preparation method thereof |
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