CN107987559A - A kind of spherical compound superfine red ceramic paint and preparation method thereof - Google Patents
A kind of spherical compound superfine red ceramic paint and preparation method thereof Download PDFInfo
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- CN107987559A CN107987559A CN201711267114.2A CN201711267114A CN107987559A CN 107987559 A CN107987559 A CN 107987559A CN 201711267114 A CN201711267114 A CN 201711267114A CN 107987559 A CN107987559 A CN 107987559A
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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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
Abstract
The invention belongs to ceramic paint technical field, and in particular to a kind of preparation method of compound superfine red ceramic paint, is specially：By a certain amount of LaFexEu1‑xO3It is added to mixed solution (0.12g P123, 50ml absolute ethyl alcohols and 0.4ml deionized waters) in, add a certain amount of butyl titanate it is to be mixed uniformly when ammonium hydroxide be added dropwise dropwise adjust pH.Stirred with certain speed, stand certain time, then collect product, and respectively washed three times with water and absolute ethyl alcohol respectively.It is dry, then calcine to remove removing template, product grinding has been obtained into red ceramic color.The compound superfine red ceramic paint that gained is prepared using the method for the present invention combines LaFexEu1‑xO3And TiO2Excellent performance, there is bright-colored, high near infrared reflectivity and high chemical stability.
Description
Technical field
The invention belongs to ceramic paint technical field, and in particular to a kind of compound superfine red ceramic paint and its preparation
Method.
Background technology
Red wavelength is about 630~750nm, is one of three primary colors and psychological primary similar to the color of new blood.
Traditional high near-infrared reflection pigment is detrimental to health first mostly containing the toxic element such as Pb, Cr and pollutes environment；Secondly
They show light color and sunlight can be reflected, produced " light pollution " mostly；They last stability and durability
Poorly, it is easy to fall off, and used a period of time reflectivity to substantially reduce.And the pigment of traditional single performance cannot expire
The demand of sufficient all trades and professions.It is just unrivaled with conventional material at the same time it is known that when material particle size drops to nanoscale
Superior function.Therefore, it is directed to synthesizing a kind of small granularity, good dispersion, bright-colored, stability with the method for green energy conservation
Good and with high near infrared reflectivity compound superfine red ceramic paint has extremely important meaning.
TiO2Have a very high near infrared emission rate, reflectivity it is very high but it the shortcomings that be to be also easy to produce " light pollution ", institute
It is few to be applied in coating material.Again from literature, compound TiO2Coating is substantially than no TiO2Coating infrared external reflection
Rate is high；In addition, from visual effect, color pigment people's more deeper than Chinese white likes.So seek at present
A kind of method of green energy conservation synthesizes the functional pigment that product particle size is small, weatherability is high, bright in luster, near infrared reflectivity is high
It is most important.
201410263554.0 patent application of Application No. discloses a kind of dark red with high near-infrared radiation reflectivity
Color non-toxic pigment and preparation method thereof, belongs to functional pigment technical field.The process employs coprecipitation, having for preparation is anti-
It is simple, easily operated to penetrate equipment needed for the pigment production of infra red radiation function, is adapted to large-scale industrial production, it is anti-in near-infrared
Its spectrum average reflectance of area is penetrated more than 68%.And pigment prepared by this method is free of organic solvent, there is safe and non-toxic, change
Learn property to stablize, easily long-term the advantages that preserving.Shortcoming is：Production cost is high, the addition of precipitating reagent may spend localized rich
Height, produces reunion or composition is not uniform enough, and calcining heat is high and calcination time length is unfavorable for energy-saving and emission-reduction.
The content of the invention
Present invention aims to overcome that defect existing in the prior art, there is provided a kind of inorganic-organic hybrid type is superfine red
The preparation method of ceramic paint, by active TiO2With red pigment LaFexEu1-xO3It is for composite, synthesize at a lower temperature
Red environment friendly inorganic pigment easy to operate, chemical stability is high.
The technical scheme is that：
A kind of preparation method of spherical compound superfine red ceramic paint, it includes the following steps：
1) by 0.1g LaFexEu1-xO3Add by P123, absolute ethyl alcohol and deionized water composition mixed solution in, it is described
In mixed solution, P123Content be 0.12g, the content of absolute ethyl alcohol is 50ml, the content of deionized water is 0.4ml；
In described matrix LaFexEu1-xO3In pigment powder, the volume of the Eu is 0~0.2, i.e. the value range of x is
0.8~1.0；Dramatically increased when when the volume of Eu is more than 0.2, not significantly improving, and mass producing to the colour generation of product
Cost；
2) butyl titanate of 0.4ml is added, ammonium hydroxide is added dropwise dropwise when to be mixed uniform adjusts pH to 7.0~9.0；
3) stirred with the speed of 100~500r/min, stand a period of time, then collect product, and use water and nothing respectively
Water-ethanol is respectively washed three times；
4) it is dry, calcine to remove removing template, product grinding is just obtained into red ceramic color.
Further, in such scheme, the stirring condition in the step 3) is：50~70 DEG C of stirring 3-5h；Stand
Time is 24~48h.
Preferably, in such scheme, the pH=8.0 in the step 2), pH are adjusted by the way that ammonium hydroxide is added dropwise, through reality
Issue after examination and approval existing pH be extremely difficult to 9.0 and more than, the dispersiveness of product and colour generation are preferable than other during pH=8.
Further, in such scheme, the drying temperature in the step 4) is 70 DEG C.
Further, in such scheme, the calcination condition in the step 4) is：300~500 DEG C of calcining 30min.Forge
When burning temperature less than 300 DEG C, reaction is insufficient, and it is impure to show as color；When calcining heat is higher than 500 DEG C, do not significantly improve
The dispersiveness and colour generation of product, if energy consumption will greatly increase during large-scale production, are unfavorable for energy-saving and emission-reduction.
Further, in such scheme, the LaFe described in step 1)xEu1-xO3Obtained through following methods：First with ten thousand
/ mono- balance weighs 9g glycine and is dissolved in 150~200ml deionized waters, is stirred on magnetic stirring apparatus, sequentially adds nitre
Sour lanthanum, ferric nitrate, europium nitrate, are stirred 110 minutes, the La (NO added3)3·6H2O、Fe(NO3)3.9H2O、Eu(NO3)3.6H2O is respectively in terms of La, Fe, Eu, glycine：(La+Fe+Eu) molar ratio is 2：1；Heated afterwards on universal electric furnace, liquid
Expanded rapidly when being evaporated soon, and discharge gas, generate fluffy powder i.e. presoma, then presoma is calcined, is ground, that is, obtained
Matrix LaFexEu1-xO3Pigment powder
Further, the La (NO of the addition3)3·6H2O、Fe(NO3)3.9H2O、Eu(NO3)3.6H2O is respectively：La
(NO3)3·6H2O 8.66g、Fe(NO3)3.9H26.87~7.68g of O, Eu (NO3)3.6H2O0.45~1.34g.
Further, the whipping temp on magnetic stirring apparatus is 50~70 DEG C.
Further, the calcining heat of the presoma is 700~900 DEG C, calcination time 4h.
Further, the calcining heat of the presoma is 750~850 DEG C.Calcining heat for 700~750 DEG C and
At 850~900 DEG C, the dispersiveness and colour generation of product are general；When calcining heat is 750~850 DEG C, the dispersiveness of product and it is in
Color is preferable.
The beneficial effects of the invention are as follows：The present invention is by LaFexEu1-xO3Red pigment and TiO2It is compound, form core shell structure.
TiO2There is high near infrared reflectivity, but be also easy to produce " light pollution "；LaFexEu1-xO3It is red pigment, belongs to perovskite knot
Structure, there is high chemical stability.Therefore it is desirable that the two advantage is combined, reach " cooperative effect ".The present invention causes
Power in a kind of method using green energy conservation synthesize a kind of granularity it is small, it is dispersed it is high, nontoxic or even less toxic, technique it is simple it is controllable,
High, the bright-colored and high chemical stability compound superfine red ceramic paint of near infrared reflectivity.
Fig. 1 is same volume (LaFe0.85Eu0.15O3) matrix under different calcining heat X-ray diffraction spectrogram；From a to
Respectively 700 DEG C, 750 DEG C, 800 DEG C, 850 DEG C, 900 DEG C；
Fig. 2 is the X-ray diffraction spectrogram of same calcining heat (750 DEG C) different addition quantity matrix；It is respectively x=from a to e
1.00th, x=0.95, x=0.90, x=0.85, x=0.80；
Fig. 3 is more excellent matrix (LaFe0.85Eu0.15O3750 DEG C of calcining heat) cladding TiO2Front and rear X-ray diffractogram；
Fig. 4 is the more excellent matrix (LaFe of 50000 times of amplification0.85Eu0.15O3750 DEG C of calcining heat) cladding TiO2Front and rear production
The SEM figures of thing；
Fig. 5 is more excellent matrix (LaFe0.85Eu0.15O3750 DEG C of calcining heat) cladding TiO2The EDS spot scan figures of product afterwards；
Fig. 6 is more excellent matrix (LaFe0.85Eu0.15O3750 DEG C of calcining heat) cladding TiO2The EDS Surface scan figures of product afterwards；
Fig. 7 is the more excellent matrix (LaFe of different amplification0.85Eu0.15O3750 DEG C of calcining heat) cladding TiO2Product afterwards
TEM figure.
Embodiment
Technical scheme is further discussed in detail with reference to embodiments, but protection scope of the present invention
It is not limited thereto.
LaFexEu1-xO3Preparation example 1 (x=0.95,750 DEG C)
150ml distilled water is poured into beaker first, temperature is placed on and is set as stirring on 60 DEG C of magnetic stirring apparatus, adds 9g
Glycine, sequentially add the La (NO of 8.66g3)3·6H2O, the Fe (NO of 7.68g3)3.9H2O, the Eu (NO of 0.45g3)3.6H2O, is stirred 110 minutes, is then placed in universal electric furnace heating, is expanded rapidly when liquid is evaporated soon, and discharges gas, is generated
Fluffy red powder, that is, presoma, then obtained presoma is calcined.Then 750 DEG C of calcining 4h, grinding obtain matrix
LaFexEu1-xO3Pigment powder.
LaFexEu1-xO3Preparation example 2 (x=0.85,750 DEG C)
180ml distilled water is poured into beaker first, temperature is placed on and is set as stirring on 60 DEG C of magnetic stirring apparatus, adds 9g
Glycine, sequentially add the La (NO of 8.66g3)3·6H2O, the Fe (NO of 6.87g3)3.9H2O, the Eu (NO of 1.34g3)3.6H2O, is stirred 110 minutes, is then placed in universal electric furnace heating, is expanded rapidly when liquid is evaporated soon, and discharges gas, is generated
Fluffy red powder, that is, presoma, then obtained presoma is calcined.Then 750 DEG C of calcining 4h, grinding obtain matrix
LaFexEu1-xO3Pigment powder.
LaFexEu1-xO3Preparation example 3 (x=0.85,700 DEG C)
200ml distilled water is poured into beaker first, temperature is placed on and is set as stirring on 60 DEG C of magnetic stirring apparatus, adds 9g
Glycine, sequentially add the La (NO of 8.66g3)3·6H2O, the Fe (NO of 6.87g3)3.9H2O, the Eu (NO of 1.34g3)3.6H2O, is stirred 110 minutes, is then placed in universal electric furnace heating, is expanded rapidly when liquid is evaporated soon, and discharges gas, is generated
Fluffy red powder, that is, presoma, then obtained presoma is calcined.Then 700 DEG C of calcining 4h, grinding obtain matrix
LaFexEu1-xO3Pigment powder.
LaFexEu1-xO3Preparation example 4 (x=0.85,750 DEG C)
The glycine for weighing 9g with a ten thousandth balance first is dissolved in the deionized water of 200ml, on magnetic stirring apparatus
Stirring, whipping temp are 70 DEG C, sequentially add lanthanum nitrate, ferric nitrate, europium nitrate, the La (NO added3)3·6H2O、Fe
(NO3)3.9H2O、Eu(NO3)3.6H2O is respectively：La(NO3)3·6H2O 8.66g、Fe(NO3)3.9H2O 6.87g、Eu(NO3)3.6H2O 1.34g, heat in universal electric furnace, are expanded rapidly when liquid is evaporated soon afterwards, and discharge gas, generate fluffy red
Powder, that is, presoma, then obtained presoma is calcined, calcining heat is 750 DEG C, calcination time 4h, and grinding, that is, obtain base
Body LaFexEu1-xO3Pigment powder.
LaFexEu1-xO3Preparation example 5 (x=0.85,800 DEG C)
The glycine for weighing 9g with a ten thousandth balance first is dissolved in the deionized water of 200ml, on magnetic stirring apparatus
Stirring, whipping temp are 70 DEG C, sequentially add lanthanum nitrate, ferric nitrate, europium nitrate, the La (NO added3)3·6H2O、Fe
(NO3)3.9H2O、Eu(NO3)3.6H2O is respectively：La(NO3)3·6H2O 8.66g、Fe(NO3)3.9H2O 6.87g、Eu(NO3)3.6H2O 1.34g, heat in universal electric furnace, are expanded rapidly when liquid is evaporated soon afterwards, and discharge gas, generate fluffy red
Powder, that is, presoma, then obtained presoma is calcined, calcining heat is 800 DEG C, calcination time 4h, and grinding, that is, obtain base
Body LaFexEu1-xO3Pigment powder.
By the matrix (LaFe of the gained of preparation example 10.95Eu0.05O3750 DEG C of calcining heat) it is compound for following embodiments 1
The preparation of superfine red ceramic paint：
Embodiment 1
A kind of preparation method of compound superfine red ceramic paint, it includes the following steps：
1) by the LaFe of 0.1gxEu1-xO3It is added to by P123, absolute ethyl alcohol and deionized water composition mixed solution in, institute
State in mixed solution, P123Content be 0.12g, the content of absolute ethyl alcohol is 50ml, and the content of deionized water is 0.4ml；
2) butyl titanate of 0.4ml is added, when to be mixed uniform, ammonium hydroxide is added dropwise dropwise and adjusts pH to 7.0~9.0；
3) stirred with the speed of 100r/min, 50 DEG C of stirring 3h；Time of repose is 24h, then collects product, and use respectively
Water and absolute ethyl alcohol are respectively washed three times；
4) 70 DEG C of dryings, 300 DEG C of calcining 30min, to remove removing template, red ceramic color has just been obtained by product grinding.
By the matrix (LaFe of the gained of preparation example 20.85Eu0.15O3750 DEG C of calcining heat) it is compound for following embodiments 2
The preparation of superfine red ceramic paint：
Embodiment 2
A kind of preparation method of compound superfine red ceramic paint, it includes the following steps：
1) by the LaFe of 0.1gxEu1-xO3It is added to by P123, absolute ethyl alcohol and deionized water composition mixed solution in, institute
State in mixed solution, P123Content be 0.12g, the content of absolute ethyl alcohol is 50ml, and the content of deionized water is 0.4ml；
2) butyl titanate of 0.4ml is added, when to be mixed uniform, ammonium hydroxide is added dropwise dropwise and adjusts pH to 8.0；
3) stirred with the speed of 300r/min, 50 DEG C of stirring 3h；Time of repose is 24h, then collects product, and use respectively
Water and absolute ethyl alcohol are respectively washed three times；
4) 70 DEG C of dryings, 400 DEG C of calcining 30min, to remove removing template, red ceramic color has just been obtained by product grinding.
By the matrix (LaFe of the gained of preparation example 30.85Eu0.15O3700 DEG C of calcining heat) it is compound for following embodiments 3
The preparation of superfine red ceramic paint：
Embodiment 3
A kind of preparation method of compound superfine red ceramic paint, it includes the following steps：
1) by the LaFe of 0.1gxEu1-xO3It is added to by P123, absolute ethyl alcohol and deionized water composition mixed solution in, institute
State in mixed solution, P123Content be 0.12g, the content of absolute ethyl alcohol is 50ml, and the content of deionized water is 0.4ml；
2) butyl titanate of 0.4ml is added, when to be mixed uniform, ammonium hydroxide is added dropwise dropwise and adjusts pH to 9.0；
3) stirred with the speed of 500r/min, 50 DEG C of stirring 3h；Time of repose is 24h, then collects product, and use respectively
Water and absolute ethyl alcohol are respectively washed three times；
4) 70 DEG C of dryings, 500 DEG C of calcining 30min, to remove removing template, red ceramic color has just been obtained by product grinding.
By the matrix (LaFe of the gained of preparation example 40.85Eu0.15O3750 DEG C of calcining heat) it is compound for following embodiments 4
The preparation of superfine red ceramic paint：
A kind of preparation method of compound superfine red ceramic paint, it includes the following steps：
1) by the LaFe of 0.1g0.85Eu0.15O3It is dissolved in mixed solution (0.12gP123, absolute ethyl alcohol 50ml, deionized water
In 0.4ml)；
2) being not added with ammonium hydroxide makes pH be 7, and the butyl titanate of 0.4ml is added dropwise dropwise afterwards, 3h is stirred at 60 DEG C；
3) 24h is stood, product is collected and is respectively washed 3 times with water and absolute ethyl alcohol；
4) it is dry at 70 DEG C；
5) 30min is calcined at 400 DEG C to go removing template to obtain compound superfine red ceramic paint.
By the matrix (LaFe of the gained of preparation example 50.85Eu0.15O3800 DEG C of calcining heat) it is compound for following embodiments 5
The preparation of superfine red ceramic paint：
A kind of preparation method of compound superfine red ceramic paint, it includes the following steps：
2) by the LaFe of 0.1g0.85Eu0.15O3It is dissolved in mixed solution (0.12gP123, absolute ethyl alcohol 50ml, deionized water
In 0.4ml)；
2) appropriate ammonium hydroxide, which is added dropwise, makes pH be 8, and the butyl titanate of 0.4ml is added dropwise dropwise afterwards, 3h is stirred at 60 DEG C；
3) 24h is stood, product is collected and is respectively washed 3 times with water and absolute ethyl alcohol；
4) it is dry at 70 DEG C；
5) 30min is calcined at 400 DEG C to go removing template to obtain compound superfine red ceramic paint.
XRD is tested
Fig. 1 is same volume LaFe0.85Eu0.15O3The X-ray diffraction spectrogram of matrix under different calcination temperatures, Fig. 1's
(a) understood with (b) contrast, 700 DEG C of whens have generated characteristic peak, and the matrix crystal form at a temperature of 700 DEG C and 750 DEG C two kinds is basic
Upper the same, the matrix characteristics peak intensity of 750 DEG C of calcinings is more slightly higher than the matrix at 700 DEG C, and characteristic peak is more sharp.The 5 of comparison diagram 1 again
LaFe under a figure can be clearly seen to five temperature0.85Eu0.15O3Characteristic peak positions are the same, and crystal form is roughly the same, and 750 DEG C are forged
The matrix peak intensity of burning is slightly above the matrix of other temperature calcinations.Fig. 2 is that the X of same 750 DEG C of different addition quantity matrixes of calcining heat is penetrated
Line diffraction spectrogram, from Fig. 2 (a) it can be seen that LaFeO3Characteristic peak it is more sharp, the larger crystallinity of peak intensity is pretty good.Again will figure
2 (a) and (b) contrast, it will be apparent that see LaFe0.95Eu0.05O3Peak intensity does not have LaFeO3Good but overall crystal form it is constant.
This is because being doped with Eu, LaFeO is caused3The distortion of crystal structure, so cause feature peak intensity to diminish, but because Eu
Solid solution is generated after incorporation, so crystal structure does not change, corresponding to each peak in XRD diagram θ all.From figure
2 (b) and (c) can know that, increase that influence of the volume of Eu to characteristic peak is little, and crystal form does not also change substantially.By to 2
(b), it is little to understand that increase volume influences cadmium ferrite structure by (c) (d) and (e), and when the volume of Eu is 0.15, characteristic peak it is strong
Degree is compared compared with other volumes, and characteristic peak is slightly better.So LaFexEu1-xO3(x=0.15), i.e., the volume of Eu be 0.15 when compared with
To be suitable.As known from the above, when calcining heat is 750 DEG C, the matrix when volume of Eu is 0.15 is more excellent matrix.
Fig. 3 is more excellent matrix (LaFe0.85Eu0.15O3750 DEG C of calcining heat) the front and rear X-ray diffractogram of cladding, see Fig. 3
(a) understand, the peak value of matrix is higher, and crystallinity is preferable；LaFe after coating is understood by Fig. 3 (b) again0.85Eu0.15O3Characteristic peak it is bright
It is aobvious to die down, TiO2Characteristic peak become top, this shows TiO2Successfully it has been coated on outside matrix.
SEM is tested
Fig. 4 (a), (b) are the more excellent matrix (LaFe of 750 DEG C of calcinings of 50000 times of amplification respectively0.85Eu0.15O3) and TiO2
The front and rear SEM figures of cladding.Understood according to Fig. 4 (a), the overall dispersiveness of matrix is relatively preferable before cladding, show spheroidal or
Approximate spheroidal.Again from Fig. 4 (b), particle is more mellow and fuller after cladding, and spherical granules are more, and dispersiveness is also more preferable,
The Expected Results of spheroidal is substantially achieved.As for TiO2Cladding situation then need further to be studied by TEM.
EDS is tested
Fig. 5 is more excellent matrix (LaFe0.85Eu0.15O3750 DEG C of calcining heat) and TiO2The EDS spot scans of product after cladding
Figure, as shown in Figure 5, sample is made of tetra- kinds of elements of O, K, Fe, Eu, and the content of O is more than LaFe0.85Eu0.15O3In O contain
Amount, this is because TiO2It has been coated on outside matrix, so the content of O increases.Not having La, this is probably to be covered by core
Inside shell.More excellent matrix (the LaFe of Fig. 6 are seen again0.85Eu0.15O3750 DEG C of calcining heat) and TiO2The EDS Surface scans of product after cladding
Figure understands that sample is made of tetra- kinds of elements of La, Eu, O, Fe, and various elements are evenly distributed.
TEM is tested
Fig. 7 (a) and (b) are the LaFe of 750 DEG C of calcining respectively0.85Eu0.15O3@TiO2Amplify under conditions of pH=8
40000 times and 400000 times of TEM figures, from 40000 times of the amplification figure of Fig. 7 (a) it will be seen that even particle distribution,
Grain is complete, and the figure of 400000 times of the amplification of Fig. 7 (a) is apparent to show deep outer shallow Expected Results in round pie and color.Face
Color depth is to calcine 750 DEG C of LaFe0.85Eu0.15O3Matrix shell structure, peripheral color it is shallow be cladding TiO2Nuclear structure, can
To find out TiO2It has been uniformly coated on matrix surface.
The mechanism of the present invention is as follows：
TiO2There is very high near infrared reflectivity, but it is also easy to produce " light pollution ", and with TiO2For the light color of color stuffing
Coating system prepared by series pigments shows light colour more, it is impossible to meets the needs of people are to color.So the present invention will have
High chemical stability, red Ca-Ti ore type material LaFexEu1-xO3With the TiO with high near infrared reflectivity2Combine,
Reach cooperative effect.Be directed to a kind of energy saving green method synthesize a kind of small granularity, good dispersion, low toxicity in addition it is nontoxic,
Near infrared reflectivity is high, and does not produce " light pollution " and bright-colored, the good compound superfine red ceramic paint of chemical stabilization.
Claims (10)
1. a kind of preparation method of spherical compound superfine red ceramic paint, it is characterised in that include the following steps：
1) by 0.1g LaFexEu1-xO3It is added to by P123, absolute ethyl alcohol and deionized water composition mixed solution in, it is described mixed
Close in solution, P123Content be 0.12g, the content of absolute ethyl alcohol is 50ml, and the content of deionized water is 0.4ml；In the base
Body LaFexEu1-xO3In pigment powder, the volume of the Eu is 0~0.2, i.e., the value range of x is 0.8~1.0；
2) butyl titanate of 0.4ml is added, ammonium hydroxide is added dropwise dropwise when to be mixed uniform adjusts pH to 7.0~9.0；
3) stirred with the speed of 100~500r/min, stand a period of time, then collect product, and use water and anhydrous second respectively
Alcohol is respectively washed three times；
4) it is dry, calcine to remove removing template, product grinding has just been obtained into red ceramic color.
2. the preparation method of compound superfine red ceramic paint according to claim 1, it is characterised in that the step 3)
In stirring condition be：50~70 DEG C of stirring 3-5h；Time of repose is 24~48h.
A kind of 3. preparation method of spherical compound superfine red ceramic paint according to claim 1, it is characterised in that
Drying temperature in the step 4) is 70 DEG C.
A kind of 4. preparation method of spherical compound superfine red ceramic paint according to claim 1, it is characterised in that
Calcination condition in the step 4) is：300~500 DEG C of calcining 30min.
A kind of 5. preparation method of compound superfine red ceramic paint according to claim 1, it is characterised in that step
1) LaFe described inxEu1-xO3Obtained through following methods：First with a ten thousandth balance weigh 9g glycine be dissolved in 150~
In 200ml deionized waters, stirred on magnetic stirring apparatus, sequentially add lanthanum nitrate, ferric nitrate, europium nitrate, stir 110 points
Clock, the La (NO added3)3·6H2O、Fe(NO3)3.9H2O、Eu(NO3)3.6H2O is respectively in terms of La, Fe, Eu, glycine：(La
+ Fe+Eu) molar ratio be 2：1；Heat on universal electric furnace, expanded rapidly when liquid is evaporated soon afterwards, and discharge gas, it is raw
Into fluffy powder, that is, presoma, then by obtained presoma calcining, grinding, that is, obtain matrix LaFexEu1-xO3Pigment powder.
A kind of 6. preparation method of spherical compound superfine red ceramic paint according to claim 5, it is characterised in that
La (the NO of the addition3)3·6H2O、Fe(NO3)3.9H2O、Eu(NO3)3.6H2O is respectively：La(NO3)3·6H2O 8.66g、
Fe(NO3)3.9H26.87~7.68g of O, Eu (NO3)3.6H20.45~1.34g of O.
A kind of 7. preparation method of spherical compound superfine red ceramic paint according to claim 5, it is characterised in that
The whipping temp on magnetic stirring apparatus is 50~70 DEG C.
A kind of 8. preparation method of spherical compound superfine red ceramic paint according to claim 5, it is characterised in that
The calcining heat of the presoma is 700~900 DEG C, calcination time 4h.
A kind of 9. preparation method of spherical compound superfine red ceramic paint according to claim 5, it is characterised in that
The calcining heat of the presoma is 700~900 DEG C.
10. a kind of preparation method of spherical compound superfine red ceramic paint according to claim 5, its feature exist
In the calcining heat of the presoma is 750~850 DEG C.
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