CN108862294A - A kind of nanometer of praseodymium zirconium yellow material and preparation method thereof - Google Patents
A kind of nanometer of praseodymium zirconium yellow material and preparation method thereof Download PDFInfo
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- CN108862294A CN108862294A CN201710317988.8A CN201710317988A CN108862294A CN 108862294 A CN108862294 A CN 108862294A CN 201710317988 A CN201710317988 A CN 201710317988A CN 108862294 A CN108862294 A CN 108862294A
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Abstract
The present invention relates to a kind of nanometer of praseodymium zirconium yellow material and preparation method thereof, including：Praseodymium nitrate, soluble silicon source aqueous solution and soluble zirconium source aqueous solution are uniformly mixed, mixed solution is obtained；The pH value of mixed solution obtained by adjusting is to 6~8, hydro-thermal reaction 10~20 hours at 180~240 DEG C, then is filtered, dried, and hydrothermal product is obtained；By gained hydrothermal product at 800~1200 DEG C after high-temperature heat treatment 1~4 hour, then it is ground, obtain the nanometer praseodymium zirconium yellow material.The praseodymium zirconium yellow material that the present invention is prepared, partial size is Nano grade, and stable homogeneous, regular crystal forms, colour generation is vivid, and application field is extensive.
Description
Technical field
The present invention relates to a kind of ceramic pigment, mainly a kind of nanoscale pr-yellow material and preparation method thereof.
Background technique
Ceramic pigment is also referred to as ceramic paint, belongs to one kind of inorganic pigment, typically refers to be resistant to high-temperature process, color development
Main body is a kind of coloring material of inorganic compound, is the important materials of ceramic coloring and incrustation.High-temperature stability and it is in
Color ability is to measure two basic foundations of ceramic pigment performance.
Zirconia-based pigment is widely used in all kinds of due to having excellent physical and chemical performance, and pure color, strong coloring force
In ceramic decoration material.Wherein, praseodymium doped zirconium silicate is a kind of yellow uitramarine environment-protecting and non-poisonous, colour generation is distinct and cost performance is high,
The high temperature as needed for can bear muffle painting technique again, receives all the time and greatly pays close attention to.
Solid reaction process is that praseodymium zirconium Huang produces most traditional method.Application for a patent for invention publication No. CN105777196A is disclosed
A kind of preparation method of pr-yellow material obtains modified electric-melting zirconia by grinding, being homogenized processing and addition reactive adhesive,
Modified zirconium oxide is recycled to react to obtain pr-yellow material resistant to high temperature with other raw material solid phases.But ceramic ink jet printing fills in recent years
The appearance of the technologies such as decorations, to the performance of conventional high-temperature colorant, more stringent requirements are proposed.Not only need colorant degree of staining high, but also
Plug nozzle in order to prevent, it is desirable to which product size is small, uniform particle diameter.Pr-yellow material partial size made from dinectly bruning is big, secondary to grind
Mill then can extreme influence hair color effect, meanwhile, the addition of mineralizer can make generation zirconium silicate crystal phase it is impure, it is also possible to can reduce
The saggar service life.
Wet chemistry method is gradually taken seriously in terms of the ceramic pigment powder for preparing high pure and ultra-fine.Application for a patent for invention is announced
Number CN104445227A discloses a kind of method that liquid-phase precipitation prepares praseodymium yellow pigments, and raw material is living on alcohols solvent, water and surface
It is reacted in the alkaline mixed solution of property agent, obtains sediment, be then spray-dried and calcine to obtain the praseodymium yellow pigments of uniform component.
But some toxic organic solvents are used in the preparation process, and reaction environment is alkalinity, is detrimental to health, pollute environment, it is difficult
For producing in enormous quantities.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of preparation method of nanoscale praseodymium zirconium yellow material, does not add mine
Agent, mild condition, environment-friendly high-efficiency, obtained colorant partial size is small, stable homogeneous, the pure distinctness of colour generation.
On the one hand, the present invention provides the preparation methods of a kind of nanometer of praseodymium zirconium yellow material, including：
Praseodymium nitrate, soluble silicon source aqueous solution and soluble zirconium source aqueous solution are uniformly mixed, mixed solution is obtained；
The pH value of mixed solution obtained by adjusting is to 6~8, hydro-thermal reaction 10~20 hours at 180~240 DEG C, then is filtered, done
It is dry, obtain hydrothermal product；
By gained hydrothermal product at 800~1200 DEG C after high-temperature heat treatment 1~4 hour, then it is ground, obtain the nanometer praseodymium
Zirconium yellow material.
The present invention obtains mixed solution after mixing using praseodymium nitrate, soluble silicon source and soluble zirconium source as raw material.It adjusts
The pH value of section gained mixed solution, so that zirconium silicate crystal structure is complete, is conducive to displacement of the praseodymium element in crystal to 6~8
Doping, and then guarantee the chromophoric characteristic of pr-yellow material.Then carry out hydro-thermal reaction processing (hydro-thermal reaction 10 at 180~240 DEG C~
20 hours), using water as medium, according to dissolution-recrystallization mechanism, formation and the crystalline substance of nucleus can be effectively controlled under liquid phase environment
The growth of grain, the praseodymium yellow pigments of synthesis nanoscale and partial size it is relatively uniform.Subsequent high-temperature heat treatment then promotes praseodymium element
Utmostly color development and the development of praseodymium zirconium citrine lattice are complete, that is to say, that it is complete to be conducive to colour developing element doping, and without adding mine
Agent guarantees that colorant is pure.
Preferably, praseodymium nitrate is added in soluble silicon source aqueous solution, it is water-soluble that soluble zirconium source is added after evenly mixing
Liquid obtains mixed solution.This order of addition can effectively prevent silicate ion to hydrolyze to form colloidal silicic acid, influence reaction effect
Fruit, and can help to subsequent thoroughly react to obtain tetragonal phase zirconium silicate with zirconium ion.
Preferably, the solubility silicon source is selected from sodium metasilicate or/and potassium silicate.
Preferably, the soluble zirconium source in zirconium nitrate, zirconyl nitrate, basic zirconium chloride and zirconium chloride at least one
Kind.
Preferably, the concentration of soluble zirconium source aqueous solution or/and soluble silicon source aqueous solution is 0.1~0.5mol/
L。
Preferably, the molar ratio of silicon, zirconium and praseodymium is 1 in the mixed solution：(1~1.2)：(0.04~0.08), preferably
It is 1：(1~1.2)：(0.06~0.08), more preferably 1:1：(0.06~0.08) and 1:1.2：(0.07~0.08).
Preferably, using alkali adjust gained mixed solution pH value, the alkali be sodium hydroxide, ammonium hydroxide, potassium hydroxide and
At least one of sodium bicarbonate.
Preferably, adjusting the pH value of gained mixed solution to 6.5~7.5.Mild friendly neutral reaction environment similarly hereinafter
When can guarantee colorant be optimal color generation property.
On the other hand, the invention of this hair additionally provides a kind of nanometer praseodymium zirconium yellow material prepared according to the above method, described to receive
The partial size of rice praseodymium zirconium yellow material is less than 500nm, preferably smaller than 200nm.
The present invention has the advantages that：
The preparation method of praseodymium zirconium yellow material provided by the invention, raw materials used simple and easy to get, solvent environment is friendly, reaction condition temperature
With it is easily-controllable, consume energy it is low, be suitble to industrialized production；
The preparation method of praseodymium zirconium yellow material provided by the invention can effectively control grain growth by hydrothermal synthesis, subsequent
It is complete that heat treatment is then conducive to colour developing element doping, and without adding mineralizer, guarantees that colorant is pure, use in whole process
Advantages of nontoxic raw materials evil, it is environmental-friendly；
The praseodymium zirconium yellow material that the present invention is prepared, partial size is Nano grade, and stable homogeneous, regular crystal forms, colour generation is vivid, application
Field is extensive.
Specific embodiment
The present invention is further illustrated below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, is not intended to limit the present invention.
The present invention prepares mixed solution and adjusts reaction environment using soluble silicon source, soluble zirconium source, praseodymium oxide as raw material
For neutrality, after pH value of solution to be mixed remains unchanged 15min, it is placed in water heating kettle and carries out hydro-thermal reaction, hydrothermal product is washed into drying
After carry out high-temperature heat treatment, by product milled processed after high-temperature heat treatment to get nanometer praseodymium zirconium yellow material.
Illustrate to following exemplary the preparation method of nanometer praseodymium zirconium yellow material provided by the invention.
The preparation of praseodymium nitrate.Praseodymium oxide is dissolved in nitric acid, praseodymium nitrate solution is made.
Choose certain soluble silicon source, certain density aqueous solution is prepared in soluble zirconium source respectively.The silicon ion, zirconium from
The concentration of sub- aqueous solution can be 0.1mol/L-0.5mol/L.It is described that soluble silicon source is optional is derived from sodium metasilicate or/and silicic acid
Potassium.The soluble zirconium source can be selected from zirconium nitrate, zirconyl nitrate, basic zirconium chloride or/and zirconium chloride etc..
Praseodymium nitrate solution, soluble silicon source aqueous solution and soluble zirconium source aqueous solution are uniformly mixed, mixed solution is obtained.
The mixed solution preparation sequence be preferably：Praseodymium nitrate solution is added in soluble silicon source aqueous solution (silicon ion solution),
Then in the case where being sufficiently stirred, soluble zirconium source aqueous solution (zirconium ion solution) is added in above-mentioned two water mixed solution.It is specific next
It says, first praseodymium nitrate solution, which is added, which can effectively limit silicate ion in silicon ion solution, hydrolyzes to form colloidal silicic acid, and
It can thoroughly react to obtain tetragonal phase zirconium silicate with the zirconium ion of subsequent addition.The molar ratio of silicon, zirconium and praseodymium in the mixed solution
It can be 1 for the molar ratio of silicon, zirconium and praseodymium in the mixed solution：(1~1.2)：(0.04~0.08), preferably 1：(1~
1.2)：(0.06~0.08), more preferably 1:1：(0.06~0.08) and 1:1.2：(0.07~0.08).
The pH value that mixed solution is adjusted using alkali is 6-8 (preferably 6.5-7.5), and pH value of solution to be mixed remains unchanged 15min
Afterwards, neutral reaction environment is made it have.On the one hand, under low pH, zirconium silicate crystal is uncrystallizable completely, that is, is unfavorable for praseodymium element
Doping, and then influence the color development that praseodymium yellow pigments are made, the zirconium silicate crystal of pure phase can be obtained to neutral range by increasing pH, especially with
6.5-7.5 best.On the other hand, pH is limited to neutral range, ensure that reaction is carried out under the conditions of comparatively gentle, non-
Strong acid, strong alkali environment, it is environmental-friendly.The alkali can be at least one in sodium hydroxide, ammonium hydroxide, potassium hydroxide and sodium bicarbonate
Kind.As an example, by the way that (note is slowly added dropwise：Rate of addition is generally 0.01-0.02ml/s) sodium hydroxide solution adjusting
Adjust the pH value of mixed solution.
Then the mixed solution of pH hydro-thermal reaction 10~20 hours at 180~240 DEG C will be regulated, then filtered, done
It is dry, obtain hydrothermal product.
By hydrothermal product at 800~1200 DEG C after high-temperature heat treatment 1~4 hour, then it is ground, obtain the nanometer praseodymium
Zirconium yellow material.
Preparation method provided by the invention does not add that mineralizer, condition be easily-controllable, environment-friendly high-efficiency, and it is yellow that the nanometer praseodymium zirconium is made
Colorant partial size is small (to be less than 500nm；More preferably less than 200nm), stable homogeneous, the pure distinctness of colour generation.
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright above content is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary specific value.
Embodiment 1
(1) it weighs 1.61g eight and is hydrated zirconium oxychloride, be dissolved in 50ml water, stir and 0.1mol/L zirconium oxychloride aqueous solution is made；Claim
Nine hydrated sodium metasilicate of 1.42g is taken, is dissolved in 50ml water, stirs and 0.1mol/L sodium silicate solution is made；Weigh 0.068g oxidation
Praseodymium is added dropwise concentrated nitric acid, gently stirs to obtain clear praseodymium nitrate solution.Praseodymium nitrate solution is added in sodium silicate aqueous solution, is then existed
It is sufficiently stirred down, zirconium oxychloride aqueous solution is added in above-mentioned two water mixed solution, mixed solution is made.Delay into mixed solution
It is slow that sodium hydroxide solution is added dropwise, pH=6.7 is adjusted, at least holding pH 15min is constant, obtains precursor liquid；
(2) precursor liquid is placed in water heating kettle, 220 DEG C of hydro-thermal reaction 18h；Then by hydrothermal product filtering and washing, 70 DEG C of drying
It is placed in Muffle furnace, 1000 DEG C of heat treatment 1h；Product milled processed after being heat-treated, obtains a nanometer praseodymium zirconium yellow material.
Embodiment 2
(1) it weighs 8.05g eight and is hydrated zirconium oxychloride, be dissolved in 50ml water, stir and 0.5mol/L zirconium oxychloride aqueous solution is made；Claim
Nine hydrated sodium metasilicate of 7.10g is taken, is dissolved in 50ml water, stirs and 0.5mol/L sodium silicate solution is made；Weigh 0.341g oxidation
Praseodymium is added dropwise concentrated nitric acid, gently stirs to obtain clear praseodymium nitrate solution.Praseodymium nitrate solution is added in sodium silicate aqueous solution, is then existed
It is sufficiently stirred down, zirconium oxychloride aqueous solution is added in above-mentioned two water mixed solution, mixed solution is made.Delay into mixed solution
It is slow that sodium hydroxide solution is added dropwise, pH=6.7 is adjusted, at least holding pH 15min is constant, obtains precursor liquid；
(2) precursor liquid is placed in water heating kettle, 220 DEG C of hydro-thermal reaction 18h；Then by hydrothermal product filtering and washing, 70 DEG C of drying
It is placed in Muffle furnace, 1000 DEG C of heat treatment 2h；Product milled processed after being heat-treated, obtains a nanometer praseodymium zirconium yellow material.
Embodiment 3
(1) it weighs 8.05g eight and is hydrated zirconium oxychloride, be dissolved in 50ml water, stir and 0.5mol/L zirconium oxychloride aqueous solution is made；Claim
Nine hydrated sodium metasilicate of 7.10g is taken, is dissolved in 50ml water, stirs and 0.5mol/L sodium silicate solution is made；Weigh 0.255g oxidation
Praseodymium is added dropwise concentrated nitric acid, gently stirs to obtain clear praseodymium nitrate solution.Praseodymium nitrate solution is added in sodium silicate aqueous solution, is then existed
It is sufficiently stirred down, zirconium oxychloride aqueous solution is added in above-mentioned two water mixed solution, mixed solution is made.Delay into mixed solution
It is slow that sodium hydroxide solution is added dropwise, pH=7.0 is adjusted, at least holding pH 15min is constant, obtains precursor liquid；
(2) precursor liquid is placed in water heating kettle, 220 DEG C of hydro-thermal reaction 18h；Then by hydrothermal product filtering and washing, 70 DEG C of drying
It is placed in Muffle furnace, 1000 DEG C of heat treatment 2h；Product milled processed after being heat-treated, obtains a nanometer praseodymium zirconium yellow material.
Embodiment 4
(1) it weighs 8.05g eight and is hydrated zirconium oxychloride, be dissolved in 50ml water, stir and 0.5mol/L zirconium oxychloride aqueous solution is made；Claim
Nine hydrated sodium metasilicate of 7.10g is taken, is dissolved in 50ml water, stirs and 0.5mol/L sodium silicate solution is made；Weigh 0.341g oxidation
Praseodymium is added dropwise concentrated nitric acid, gently stirs to obtain clear praseodymium nitrate solution.Praseodymium nitrate solution is added in sodium silicate aqueous solution, is then existed
It is sufficiently stirred down, zirconium oxychloride aqueous solution is added in above-mentioned two water mixed solution, mixed solution is made.Delay into mixed solution
It is slow that sodium hydroxide solution is added dropwise, pH=7.0 is adjusted, at least holding pH 15min is constant, obtains precursor liquid；
(2) precursor liquid is placed in water heating kettle, 220 DEG C of hydro-thermal reaction 18h；Then by hydrothermal product filtering and washing, 70 DEG C of drying
It is placed in Muffle furnace, 1200 DEG C of heat treatment 2h；Product milled processed after being heat-treated, obtains a nanometer praseodymium zirconium yellow material.
Embodiment 5
(1) it weighs 8.05g eight and is hydrated zirconium oxychloride, be dissolved in 50ml water, stir and 0.5mol/L zirconium oxychloride aqueous solution is made；Claim
Nine hydrated sodium metasilicate of 7.10g is taken, is dissolved in 50ml water, stirs and 0.5mol/L sodium silicate solution is made；Weigh 0.341g oxidation
Praseodymium is added dropwise concentrated nitric acid, gently stirs to obtain clear praseodymium nitrate solution.Praseodymium nitrate solution is added in sodium silicate aqueous solution, is then existed
It is sufficiently stirred down, zirconium oxychloride aqueous solution is added in above-mentioned two water mixed solution, mixed solution is made.Delay into mixed solution
It is slow that sodium hydroxide solution is added dropwise, pH=7.5 is adjusted, at least holding pH 15min is constant, obtains precursor liquid；
(2) precursor liquid is placed in water heating kettle, 220 DEG C of hydro-thermal reaction 10h；Then by hydrothermal product filtering and washing, 70 DEG C of drying
It is placed in Muffle furnace, 1200 DEG C of heat treatment 3h；Product milled processed after being heat-treated, obtains a nanometer praseodymium zirconium yellow material.
Embodiment 6
(1) it weighs 8.05g eight and is hydrated zirconium oxychloride, be dissolved in 50ml water, stir and 0.5mol/L zirconium oxychloride aqueous solution is made；Claim
Nine hydrated sodium metasilicate of 7.10g is taken, is dissolved in 50ml water, stirs and 0.5mol/L sodium silicate solution is made；Weigh 0.341g oxidation
Praseodymium is added dropwise concentrated nitric acid, gently stirs to obtain clear praseodymium nitrate solution.Praseodymium nitrate solution is added in sodium silicate aqueous solution, is then existed
It is sufficiently stirred down, zirconium oxychloride aqueous solution is added in above-mentioned two water mixed solution, mixed solution is made.Delay into mixed solution
It is slow that sodium hydroxide solution is added dropwise, pH=7.5 is adjusted, at least holding pH 15min is constant, obtains precursor liquid；
(2) precursor liquid is placed in water heating kettle, 180 DEG C of hydro-thermal reaction 20h；Then by hydrothermal product filtering and washing, 70 DEG C of drying
It is placed in Muffle furnace, 1200 DEG C of heat treatment 4h；Product milled processed after being heat-treated, obtains a nanometer praseodymium zirconium yellow material.
Embodiment 7
(1) it weighs 9.66g eight and is hydrated zirconium oxychloride, be dissolved in 60ml water, stir and 0.5mol/L zirconium oxychloride aqueous solution is made；Claim
Nine hydrated sodium metasilicate of 7.10g is taken, is dissolved in 50ml water, stirs and 0.5mol/L sodium silicate solution is made；Weigh 0.341g oxidation
Praseodymium is added dropwise concentrated nitric acid, gently stirs to obtain clear praseodymium nitrate solution.Praseodymium nitrate solution is added in sodium silicate aqueous solution, is then existed
It is sufficiently stirred down, zirconium oxychloride aqueous solution is added in above-mentioned two water mixed solution, mixed solution is made.Delay into mixed solution
It is slow that sodium hydroxide solution is added dropwise, pH=7.8 is adjusted, at least holding pH 15min is constant, obtains precursor liquid；
(2) precursor liquid is placed in water heating kettle, 220 DEG C of hydro-thermal reaction 18h；Then by hydrothermal product filtering and washing, 70 DEG C of drying
It is placed in Muffle furnace, 1200 DEG C of heat treatment 4h；Product milled processed after being heat-treated, obtains a nanometer praseodymium zirconium yellow material.
Embodiment 8
(1) it weighs 8.05g eight and is hydrated zirconium oxychloride, be dissolved in 50ml water, stir and 0.5mol/L zirconium oxychloride aqueous solution is made；Claim
Nine hydrated sodium metasilicate of 7.10g is taken, is dissolved in 50ml water, stirs and 0.5mol/L sodium silicate solution is made；Weigh 0.341g oxidation
Praseodymium is added dropwise concentrated nitric acid, gently stirs to obtain clear praseodymium nitrate solution.Praseodymium nitrate solution is added in sodium silicate aqueous solution, is then existed
It is sufficiently stirred down, zirconium oxychloride aqueous solution is added in above-mentioned two water mixed solution, mixed solution is made.Delay into mixed solution
It is slow that sodium hydroxide solution is added dropwise, pH=6.0 is adjusted, at least holding pH 15min is constant, obtains precursor liquid；
(2) precursor liquid is placed in water heating kettle, 220 DEG C of hydro-thermal reaction 18h；Then by hydrothermal product filtering and washing, 70 DEG C of drying
It is placed in Muffle furnace, 1200 DEG C of heat treatment 2h；Product milled processed after being heat-treated, obtains a nanometer praseodymium zirconium yellow material.
Embodiment 9
(1) it weighs 8.05g eight and is hydrated zirconium oxychloride, be dissolved in 50ml water, stir and 0.5mol/L zirconium oxychloride aqueous solution is made；Claim
Nine hydrated sodium metasilicate of 7.10g is taken, is dissolved in 50ml water, stirs and 0.5mol/L sodium silicate solution is made；Weigh 0.341g oxidation
Praseodymium is added dropwise concentrated nitric acid, gently stirs to obtain clear praseodymium nitrate solution.Praseodymium nitrate solution is added in sodium silicate aqueous solution, is then existed
It is sufficiently stirred down, zirconium oxychloride aqueous solution is added in above-mentioned two water mixed solution, mixed solution is made.Delay into mixed solution
It is slow that sodium hydroxide solution is added dropwise, pH=8.0 is adjusted, at least holding pH 15min is constant, obtains precursor liquid；
(2) precursor liquid is placed in water heating kettle, 220 DEG C of hydro-thermal reaction 18h；Then by hydrothermal product filtering and washing, 70 DEG C of drying
It is placed in Muffle furnace, 1200 DEG C of heat treatment 2h；Product milled processed after being heat-treated, obtains a nanometer praseodymium zirconium yellow material.
International Commission on Illumination's regulation characterizes color sample using CIE L*a*b* parameter.Wherein, b* parameter list sample
The yellowing of product, b* value is bigger, and the yellow coloration of sample is better.A* value is the redness of sample, and a* value should be as far as possible close to 0.L*
Value refers to the brightness of sample, and L* value is bigger, and close to 0, obtained sample is brighter for the absolute value of a* or b*, but sample
Whiteness is also higher, does not meet the color development requirement of colorant.Using HITACHI UH4150 UV, visible light point in the embodiment of the present invention
Light photometer tests the visible reflectance spectrum of obtained colorant and calculates CIE L*a*b* parameter.
The preparation condition and CIE L*a*b* parameter of the praseodymium zirconium yellow material provided in an embodiment of the present invention of table 1：
As shown in Table 1, the preparation method of a kind of praseodymium zirconium yellow material provided by the invention, is made sample yellowing height, and tone is pure
Just, colour generation is distinct.
Comparative example 1
(1) it weighs 8.05g eight and is hydrated zirconium oxychloride, be dissolved in 50ml water, stir and 0.5mol/L zirconium oxychloride aqueous solution is made；Claim
Nine hydrated sodium metasilicate of 7.10g is taken, is dissolved in 50ml water, stirs and 0.5mol/L sodium silicate solution is made；Weigh 0.341g oxidation
Praseodymium is added dropwise concentrated nitric acid, gently stirs to obtain clear praseodymium nitrate solution.Above-mentioned three kinds of solution is mixed simultaneously, is delayed into mixed solution
It is slow that sodium hydroxide solution is added dropwise, pH=7.0 is adjusted, at least holding pH 15min is constant, obtains precursor liquid；
(2) precursor liquid is placed in water heating kettle, 220 DEG C of hydro-thermal reaction 18h；Then by hydrothermal product filtering and washing, 70 DEG C of drying
It is placed in Muffle furnace, 1200 DEG C of heat treatment 2h；Product milled processed after being heat-treated, obtains a nanometer praseodymium zirconium yellow material；
Each component is added in this comparative example 1 simultaneously, the generation of orthosilicic acid is more difficult to get control, and presoma cohesion is glue, influences
The generation of tetragonal phase zirconium silicate crystal during follow-up hydrothermal.It is only light yellow that final product color is thus made.Test CIE
L*a*b* parameter：L*=92.1471；A*=-5.0335, b*=36.4722.
Claims (9)
1. the preparation method of a kind of nanometer of praseodymium zirconium yellow material, which is characterized in that including：
Praseodymium nitrate, soluble silicon source aqueous solution and soluble zirconium source aqueous solution are uniformly mixed, mixed solution is obtained；
The pH value of mixed solution obtained by adjusting is to 6~8, hydro-thermal reaction 10~20 hours at 180~240 DEG C, then is filtered, done
It is dry, obtain hydrothermal product；
By gained hydrothermal product at 800~1200 DEG C after high-temperature heat treatment 1~4 hour, then it is ground, obtain the nanometer praseodymium
Zirconium yellow material.
2. preparation method according to claim 1, which is characterized in that praseodymium nitrate is added in soluble silicon source aqueous solution,
Soluble zirconium source aqueous solution is added after evenly mixing, obtains mixed solution.
3. preparation method according to claim 1 or 2, which is characterized in that it is described solubility silicon source be selected from sodium metasilicate or/
And potassium silicate.
4. preparation method according to any one of claim 1-3, which is characterized in that the soluble zirconium source is selected from nitric acid
At least one of zirconium, zirconyl nitrate, basic zirconium chloride and zirconium chloride.
5. preparation method described in any one of -4 according to claim 1, which is characterized in that soluble zirconium source aqueous solution
Or/and the concentration of soluble silicon source aqueous solution is 0.1~0.5mol/L.
6. preparation method according to any one of claims 1-5, which is characterized in that silicon in the mixed solution, zirconium and
The molar ratio of praseodymium is 1：（1~1.2）：（0.04~0.08）, preferably 1：（1~1.2）：（0.06~0.08）, more preferably 1:
1：（0.06~0.08）With 1:1.2：（0.07~0.08）.
7. preparation method according to claim 1 to 6, which is characterized in that adjust gained mixed solution using alkali
PH value, the alkali is at least one of sodium hydroxide, ammonium hydroxide, potassium hydroxide and sodium bicarbonate.
8. preparation method described in any one of -7 according to claim 1, which is characterized in that adjust the pH value of gained mixed solution
To 6.5~7.5.
9. a kind of nanometer praseodymium zirconium yellow material of preparation method preparation according to claim 1 to 8, feature exist
In the partial size of the nanometer praseodymium zirconium yellow material is less than 500 nm, preferably smaller than 200 nm.
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