CN105130499B - 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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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 ceramic paint technical field, and in particular to a kind of compound ultra-fine yellow ceramic paint and its preparation
Method.
Background technology
Yellow should be the monochromatic color of wavelength 597-577nm in meaning physically, and no matter is yellow ceramic paint
It, for ceramic illuminated, or is all the ceramic decoration indispensable decoration of art as the toner of ceramic colour glaze or color embryo to be
Material.Traditional yellow uitramarine includes poisonous heavy metal such as lead, chromium etc. mostly, and to environment and individual serious shadow is caused
Ring, and the pigment of traditional single performance can not meet the demand of all trades and professions.Simultaneously it is known that when scantling is dropped to
After nanoscale, just there is the unrivaled superior function of conventional material.Therefore, the synthetic method of green is sought, in temperature relatively
Obtain that size is little, the high-performance nano yellow uitramarine of good dispersion, even particle size distribution is imperative in the environment of sum.
Conventional TiO2It is a kind of heat-insulated pigment of high infrared reflection, it is fluffy white powder, shielding ultraviolet rays effect is strong,
There is good dispersiveness and weatherability.But because its own outward appearance is white, so easily causing white pollution, air is made
Into a certain degree of pollution, the retina of people has also been injured to a certain extent.
The patent application of Application No. 201410405705.1 discloses a kind of preparation of inorganic-organic hybrid yellow uitramarine
Method, although the pigment has the advantages that heat endurance is good, good light stability, and the compound yellow uitramarine and Inorganic yellow pigment
Lead chromate yellow is compared, and shows more excellent tinctorial property, and such as tinting strength, tinting power is higher, and color is more bright-coloured, and yellow is more pure etc., but
It is the complex operation step in its preparation process, large-scale production is difficult to ensure that quality, and relatively costly；And synthesis temperature
Height, is unfavorable for industrialized production.
The content of the invention
Present invention aim to overcome that prior art defect, there is provided a kind of compound ultra-fine yellow ceramics face of inorganic-inorganic
Material and preparation method thereof, it is by active TiO2With yellow uitramarine NiTiO3It is combined, high brightness has been synthesized at a lower temperature
Yellow environment-friendly inorganic pigment.
For achieving the above object, the present invention is adopted the following technical scheme that：
A kind of preparation method of compound ultra-fine yellow ceramic paint, it comprises the steps：
1）Nickel titanate is soluble in water, obtain solution A；
2）Butyl titanate is well mixed with the absolute ethyl alcohol of 2-3 volumes times, solution B is obtained；The butyl titanate of addition with
Titanium dioxide meter, the addition of nickel titanate is 2-10 times of titanium dioxide quality；
3）Solution B is added dropwise in solution A under agitation, more than 5h, then still aging 24- is stirred at room temperature
48h obtains opaque gel；
4）Step 3）The opaque gel drying of gained, grinding obtain loose precursor powder, then proceed to Muffle furnace
In in 400-500 DEG C of roasting 4-6h, obtain final product yellow ceramic paint.
Specifically, step 3）In mixing speed be preferably 80-100 rev/min；Step 4）In drying condition be preferably：
80 DEG C are first dried 4h, then 90 DEG C are dried 2h.
Step 1）Described in nickel titanate（NiTiO3）The following methods of Jing are obtained：By Ni (NO3)2·6H2O and butyl titanate
In being added to the aqueous solution of glycine, stir to clarify at 60 ± 10 DEG C be then heated to 100-120 DEG C of stirring 100 first
± 10min, in the process solution generation self-propagating combustion reaction generates loose powder, and gained powder is forged in 700-900 DEG C
Burning is obtained final product.
In the preparation process of above-mentioned nickel titanate, the Ni (NO of addition3)2·6H2O, butyl titanate respectively in terms of Ni, Ti, sweet ammonia
Sour mole is 2 times of Ni, Ti mole sum；Calcining heat is preferably 750-850 DEG C, still more preferably 800-850
℃。
The compound ultra-fine yellow ceramic paint prepared using any of the above-described method.
In the preparation process of nickel titanate, at 700-900 DEG C, gained nickel titanate dispersiveness is general, colour generation for calcining heat
Typically；, at 750-850 DEG C, preferably, colour generation is preferable for gained nickel titanate dispersiveness for calcining heat；Calcining heat is in 800-
When 850 DEG C, preferably, colour generation is preferably also gained nickel titanate dispersiveness.
Step 3）In time preferred 5-6h is stirred at room temperature.The stirring reaction time is less than 5h, and product is not sufficiently reacted multiple
Close, cause product mutually uneven.Step 4）In, sintering temperature at 400-500 DEG C, the compound ultra-fine yellow ceramics face of gained
Preferably, size distribution is more uniform for material product dispersiveness.If calcining heat is too low（Less than 400 DEG C）, then product can not be abundant
It is compound, show as color impure；If calcining heat is too high（More than 500 DEG C）, although the colourity of product is without significant change, but work
Industry metaplasia is produced power consumption and will be greatly increased.
Compared to the prior art, beneficial effects of the present invention：
The present invention is by NiTiO3Yellow uitramarine and TiO2It is compound, by the cooperative effect of the two, the advantage of the two is performed to
Most preferably, NiTiO has been synthesized3/TiO2Nano composite ceramic pigment.Compound ultra-fine yellow ceramic paint is combined obtained by of the invention
NiTiO3And TiO2Premium properties, there is bright in colour, high temperature nondiscolouring.Additionally, preparation method letter of the present invention
Single, raw material is easy to get, and synthesis temperature is low, and process is simple is controllable, is suitable to large-scale production；And products obtained therefrom be low molecule, low toxicity very
To the toxic elements such as non-toxic organic thing, not leaded chromium, environmental protection, product particles good dispersion, even particle size distribution, colour generation
It is good.
Description of the drawings
Fig. 1 is NiTiO3X-ray diffraction spectrogram before and after compound；
Fig. 2 is TiO2Measure identical, different sintering temperatures（400、500℃）Under, embodiment 2 and 4 is compound（NiTiO3/
TiO2）The X-ray diffraction spectrogram of ultra-fine yellow ceramic paint；
Fig. 3 is the NiTiO under different calcining heats, identical multiplication factor3SEM photos；In figure, a calcining heats are
700 DEG C, b calcining heats are 800 DEG C, and c calcining heats are 900 DEG C；
Fig. 4 is the NiTiO of same multiplication factor3SEM photograph before and after compound；
Fig. 5 is NiTiO3The local Surface scan energy spectrum diagram of product after compound.
Fig. 6 is NiTiO3The energy spectrum analysis figure of product after compound.
Specific embodiment
Technical scheme is further discussed in detail with reference to embodiments, but protection scope of the present invention
It is not limited thereto.
NiTiO3Preparation example 1
30g glycine is dissolved in 100mL distilled water first, is subsequently adding the Ni (NO of 29.1g3)2·6H2O's and 34g
Butyl titanate, is placed on stirring and dissolving on the magnetic stirring apparatus that design temperature is 60 DEG C, and to dissolving clarified solution is obtained completely（About need
20min）.Be then heated to 110 DEG C reaction 100min, in the process the sticky expansion of liquid, and then discharge gas, rapidly
Generation self-propagating combustion reacts, and generates loose powder.Gained powder calcines 4h, i.e. Yellow nanometer pigment at 700 DEG C
NiTiO3。
NiTiO3Preparation example 2
30g glycine is dissolved in first the Ni (NO that 29.1g is then sequentially added in 100mL distilled water3)2·6H2O and
The butyl titanate of 34g, is placed on dissolving stirring on the magnetic stirring apparatus that design temperature is 60 DEG C, and to dissolving clarified solution is obtained completely
（About need 20min）.Be then heated to 110 DEG C reaction 100min, in the process the sticky expansion of liquid, ' discharge gas, rapidly
Generation self-propagating combustion reacts, and generates loose powder.Gained powder calcines 4h at 800 DEG C, obtains final product Yellow nanometer pigment
NiTiO3。
NiTiO3Preparation example 3
30g glycine is dissolved in during 120mL distilled water goes first, then sequentially adds the Ni (NO of 29.1g3)2·6H2O and
The butyl titanate of 34g, is placed on dissolving stirring on the magnetic stirring apparatus that design temperature is 60 DEG C, and to dissolving clarified solution is obtained completely
（About need 20min）.Be then heated to 110 DEG C reaction 100min, in the process the sticky expansion of liquid, and then discharge outlet
Body, it is rapid that self-propagating combustion reaction occurs, generate loose powder.Gained powder calcines 4h at 900 DEG C, obtains final product Yellow nanometer
Pigment NiTiO3。
By the NiTiO of the gained of preparation example 23For the preparation of following compound ultra-fine yellow ceramic paints.
Embodiment 1
A kind of preparation method of compound ultra-fine yellow ceramic paint, it comprises the steps：
1）2g nickel titanates are added in 100mL water, are stirred, obtain solution A；
2）By 0.852g butyl titanates（It is 0.2g titanium dioxide after conversion）It is well mixed with the absolute ethyl alcohol of 3 volumes times,
Obtain solution B；
3）Solution B is added dropwise in solution A under agitation, so that 6h is stirred at room temperature under 90 revs/min of speed, then
Still aging 48h obtains opaque gel；
4）Step 3）The opaque gel of gained is first dried 4h at 80 DEG C, then 90 DEG C are dried 2h, then ground to obtain loose
Precursor powder, finally proceed in Muffle furnace in 400 DEG C of roasting 5h, obtain final product compound（NiTiO3/ TiO2）Ultra-fine yellow pottery
Porcelain pigment.
Embodiment 2
A kind of preparation method of compound ultra-fine yellow ceramic paint, it comprises the steps：
1）2g nickel titanates are added in 100mL water, are stirred, obtain solution A；
2）By 3.409g butyl titanates（It is 0.8g titanium dioxide after conversion）It is well mixed with the absolute ethyl alcohol of 2 volumes times,
Obtain solution B；
3）Solution B is added dropwise in solution A under agitation, so that 5h is stirred at room temperature under 90 revs/min of speed, then
Still aging 24h obtains opaque gel；
4）Step 3）The opaque gel of gained is first dried 4h at 80 DEG C, then 90 DEG C are dried 2h, then ground to obtain loose
Precursor powder, finally proceed in Muffle furnace in 400 DEG C of roasting 5h, obtain final product compound（NiTiO3/ TiO2）Ultra-fine yellow pottery
Porcelain pigment.
Embodiment 3
A kind of preparation method of compound ultra-fine yellow ceramic paint, it comprises the steps：
1）2g nickel titanates are added in 100mL water, are stirred, obtain solution A；
2）By 0.852g butyl titanates（It is 0.2g titanium dioxide after conversion）It is well mixed with the absolute ethyl alcohol of 3 volumes times,
Obtain solution B；
3）Solution B is added dropwise in solution A under agitation, so that 6h is stirred at room temperature under 100 revs/min of speed,
Again still aging 48h obtains opaque gel；
4）Step 3）The opaque gel of gained is first dried 4h at 80 DEG C, then 90 DEG C are dried 2h, then ground to obtain loose
Precursor powder, finally proceed in Muffle furnace in 500 DEG C of roasting 5h, obtain final product compound（NiTiO3/ TiO2）Ultra-fine yellow pottery
Porcelain pigment.
Embodiment 4
A kind of preparation method of compound ultra-fine yellow ceramic paint, it comprises the steps：
1）2g nickel titanates are added in 100mL water, are stirred, obtain solution A；
2）By 3.409g butyl titanates（It is 0.8g titanium dioxide after conversion）It is well mixed with the absolute ethyl alcohol of 2 volumes times,
Obtain solution B；
3）Solution B is added dropwise in solution A under agitation, so that 5h is stirred at room temperature under 90 revs/min of speed, then
Still aging 24h obtains opaque gel；
4）Step 3）The opaque gel of gained is first dried 4h at 80 DEG C, then 90 DEG C are dried 2h, then ground to obtain loose
Precursor powder, finally proceed in Muffle furnace in 500 DEG C of roasting 5h, obtain final product compound（NiTiO3/ TiO2）Ultra-fine yellow pottery
Porcelain pigment.
XRD is tested
To pure NiTiO3It is compound with the present invention（NiTiO3/ TiO2）Ultra-fine yellow ceramic paint has carried out XRD analysis,
As shown in Figure 1.As a result understand：With pure NiTiO3Compare, the present invention is compound（NiTiO3/ TiO2）Ultra-fine yellow ceramic paint
TiO is occurred in that2Characteristic diffraction peak, it is consistent with the set goal.
Identical TiO2Amount, different sintering temperatures it is compound（NiTiO3/ TiO2）The XRD of ultra-fine yellow ceramic paint
Type, as shown in Figure 2.As a result understand：After 400 DEG C of roasting 5h, TiO has been occurred in that2Characteristic diffraction peak, continue ascending temperature
After for 500 DEG C, stronger TiO is occurred in that2Characteristic diffraction peak, is considered based on energy conservation, and preferred sintering temperature is 400 DEG C.
SEM is tested
Micro-structural test is carried out to product by ESEM, Fig. 3 is under different calcining heats, identical multiplication factor
NiTiO3SEM photos.We can be clearly seen that from photo：Matrix NiTiO3 has dispersiveness well, particle
Distribution is than more uniform.Simultaneously, it can be observed that when temperature is from 700 DEG C to 900 DEG C, the average-size of crystal grain constantly increases, particle diameter
Size in 50nm or so, in nano level scope, so the material belongs to nano material category.Fig. 4 is same multiplication factor
NiTiO3SEM photograph before and after compound, the photo explanation combination product（NiTiO3/ TiO2）Pattern ball is changed into from graininess
Shape, surface is because coating TiO2And seem that some are coarse.Compound NiTiO3/ TiO2The good dispersion of material, even particle size distribution.It is right
For pigment, granularity is less, and particle specific surface is bigger, and specific surface energy is higher, and in addition material scatter is good, in use
Uniform coating is easily formed, and adhesive force is strong, evenness.
EDS is tested
Face constituent test is carried out to product by energy disperse spectroscopy, as it can be seen in figures 5 and 6, Fig. 5 is NiTiO3/TiO2Nanometer
The Surface scan energy spectrum diagram of material, the product NiTiO after the figure explanation is compound3/ TiO2Be made up of tri- kinds of elements of element Ni, Ti, O and
Surface distributed is visibly homogeneous, chemical segregation phenomena does not occur.Fig. 6 is NiTiO3/ TiO2Energy spectrum analysis figure before and after compound, Jing
Contrast is crossed, we can become apparent from：NiTiO3The content of element Ni is significantly reduced after compound, and the content of element ti is big
It is big to increase.This explanation can make in this way activating oxide TiO2It is coated on NiTiO3On surface.Additionally, the original of Ni/Ti
Son is than being less than 1:1.This is because Jing after compound, NiTiO3Nanocrystalline to be coated by TiO2, element Ni is wrapped in a nanometer material
Material the inside, so content is reduced, and element ti is attached to particle surface, adds NiTiO3The Ti elements for itself being included, institute
Can be increased with atom content.
Colourity is tested
It is compound obtained by preparing to embodiment 1 and 2（NiTiO3/ TiO2）Ultra-fine yellow ceramic paint carries out colourity survey
Examination, the results are shown in Table 1.
Table 1 is NiTiO3With TiO2The color coordinates schematic diagram of combination product
As can be seen from Table 1：With activating oxide TiO2The increase of amount, the value of a* is in a slight decrease, and b* is from matrix
21.2 increase to 38.7.And lightness L* is being continuously increased, by 42.3 51.0 are increased to.Illustrate within the specific limits, with TiO2
The increase of content, the color of combination product more tends to glassy yellow.Wherein, L* is brightness；A* be red green changing value, the bigger expressions of a*
Product colour is redder；B* is yellowish green changing value, and b* is bigger to represent that product colour is more yellow.
The mechanism of the present invention is as follows：
NiTiO3Matrix is the perovskite structure that a class has extensive chemical stability, water insoluble, insoluble in ethanol, no
It is dissolved in acid.And TiO2It is a kind of heat-insulated pigment of high infrared reflection, but has the disadvantage the white appearance due to it, it is easy to causes " white
Light " pollutes, the retina of harm people.Therefore, the two is effectively combined, the high infrared reflection of high comprehensive performance can be combined out
Insulating color pigment.
Claims (3)
1. a kind of preparation method of compound ultra-fine yellow ceramic paint, it is characterised in that comprise the steps：
1）Nickel titanate is soluble in water, obtain solution A；
2）Butyl titanate is well mixed with the absolute ethyl alcohol of 2-3 volumes times, solution B is obtained；The butyl titanate of addition is with dioxy
Change titanium meter, the addition of nickel titanate is 2-10 times of titanium dioxide quality；
3）Solution B is added in solution A under agitation, more than 5h is stirred at room temperature, then still aging 24-48h is obtained not
Clear gel；
4）Step 3）The opaque gel drying of gained, grinding obtain loose precursor powder, then proceed in Muffle furnace in
400-500 DEG C of roasting 4-6h, obtains final product yellow ceramic paint；
Step 3）In mixing speed be 80-100 rev/min；Step 4）In drying condition be specially：80 DEG C are first dried 4h, then
90 DEG C are dried 2h；
Step 1）Described in the following methods of nickel titanate Jing obtain：By Ni (NO3)2·6H2O and butyl titanate are added to glycine
The aqueous solution in, first stir to clarify at 60 ± 10 DEG C, be then heated to 100-120 DEG C of 100 ± 10min of stirring, here mistake
In journey there is the loose powder of self-propagating combustion reaction generation in solution, and gained powder is obtained final product in 700-900 DEG C of calcining.
2. the as claimed in claim 1 preparation method of compound ultra-fine yellow ceramic paint, it is characterised in that the Ni of the addition
(NO3)2·6H2Respectively in terms of Ni, Ti, glycine mole is 2 times of Ni, Ti mole sum for O, butyl titanate；Calcining heat
For 750-850 DEG C.
3. the compound ultra-fine yellow ceramic paint for being prepared using the methods described of claim 1 or 2, it is characterised in that right
Compound NiTiO obtained by preparation3/ TiO2Ultra-fine yellow ceramic paint carries out colourity test, the results are shown in Table 1：
Table 1 is NiTiO3With TiO2The color coordinates schematic diagram of combination product
As can be seen from Table 1：With activating oxide TiO2The increase of amount, the value of a* is in a slight decrease, and b* increases from the 21.2 of matrix
To 38.7；And lightness L* is being continuously increased, by 42.3 51.0 are increased to；Illustrate within the specific limits, with TiO2The increasing of content
Plus, the color of combination product more tends to glassy yellow；Wherein, L* is brightness；A* be red green changing value, the bigger expression product colours of a*
It is redder；B* is yellowish green changing value, and b* is bigger to represent that product colour is more yellow.
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| 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 |
| CN108017936B (en) * | 2017-12-05 | 2020-07-28 | 华北水利水电大学 | Preparation method of spherical composite superfine yellow 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 |
| 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 |
| CN108929569B (en) * | 2018-08-24 | 2020-05-22 | 华北水利水电大学 | Composite red ceramic pigment LaFeO3/SiO2Preparation method of (1) |
| 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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