CN106590032A - Cerium yellow composite functional material and preparation method - Google Patents
Cerium yellow composite functional material and preparation method Download PDFInfo
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- CN106590032A CN106590032A CN201611128943.8A CN201611128943A CN106590032A CN 106590032 A CN106590032 A CN 106590032A CN 201611128943 A CN201611128943 A CN 201611128943A CN 106590032 A CN106590032 A CN 106590032A
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- cerium
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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
- C09C1/02—Compounds of alkaline earth metals or magnesium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/02—Oxides; Hydroxides
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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
-
- 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
- C09C1/36—Compounds of titanium
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention relates to a cerium yellow composite functional material and a preparation method. A molecular formula of the cerium yellow composite functional material is Ce1-xMxW2O8, wherein M is one or multiple of titanium, zirconium, calcium and bismuth, and x is greater than 0 and smaller than 1. The preparation method includes : performing liquid phase synthesis on cerate and tungstate and salt of one or multiple of titanium, zirconium, calcium and bismuth in the presence of urea; calcining a liquid phase synthesis product at 400-1000 DEG C in an oxidizing atmosphere. Cerium yellow is bright in color, has high tinting power and saturability, has high weatherability and chemical stability and is free of heavy metal, environment-friendly and nontoxic. The cerium yellow composite functional material can be widely applied in the field of paint, printing ink, plastic, ceramic and enamel.
Description
Technical field
The invention belongs to the synthesis technical field of composite functional material, and in particular to a kind of composite functional material of yellow containing cerium
And preparation method thereof.
Background technology
Yellow is situated between the color formed by 560～590 millimicrons of light by wavelength.In daily life, every need
Where wanting our hig diligences（Such as school bus, traffic signss）Will colored yellow.
Yellow organic dye, because with excellent weatherability and thermostability, leading in high-temperature molding material and construction material
Domain uses in a large number, there is also substantial amounts of demand in coating, paint, ceramic field.In the Yellow organic dye being currently known,
Chrome yellow and cadmium yellow（Cadmium sulfide）Tinting strength, tinting power is high, but contains heavy metal, environment and people is known from experience and produces damaging influence；Lanthanum sulfide
（La2S3）Meet water or acid can discharge hydrogen sulfide toxic gas；Titan yellow, titanium yellow and praseodymium yellow coloring Dipeptiven is low, plastics and coating
It is difficult with.
The content of the invention
It is an object of the invention to provide the yellow uitramarine of a kind of strong coloring force, environment-protecting asepsis.
By substantial amounts of research, molecular formula is Ce1-xMxW2O8（M in formula be titanium, zirconium, calcium, bismuth it is therein one or more,
0<x<1）Pigment be found to show bright yellow, safety non-toxic.
The technical scheme is that：A kind of cerium Huang composite functional material, molecular formula is Ce1-xMxW2O8, the M in formula is
Titanium, zirconium, calcium, bismuth it is therein one or more, 0<x<1.Preferred 0.1≤x≤0.4.
The preparation method of the cerium Huang composite functional material, by one kind in cerium salt, tungstates and titanium, zirconium, calcium, bismuth or several
The salt planted liquid phase synthesis in the presence of carbamide, then 400～1000 DEG C of calcinings in oxidizing atmosphere by liquid phase synthesis product.
The salt of titanium, zirconium, calcium or bismuth includes one or more in nitrate, sulfate, acetate and chloride.Cerium salt bag
Include one or more in nitrate, sulfate and chloride.Tungstates includes one or more in alkali tungstates.
Preferably, carbamide and cerium salt mol ratio 3 ~ 4:1.
Preferably, liquid phase synthesis pH=8～10.
Preferably, 70～100 DEG C of liquid phase synthesis temperature.
Preferably, 1～3h of liquid phase synthesis time.
Preferably, 2～4h of calcination time.
Preferably, liquid phase synthesis terminate, and first wash and the drying in 100～300 DEG C of oxidizing atmosphere product.
The present invention provide cerium Huang be a kind of new composite inorganic yellow material, there is presently no similar products research and development,
The report of production, the pigment color are bright-coloured, with high coloring power and saturation, it may have good weatherability and chemical stability,
Heavy metal, environment-protecting asepsis are not contained.Can be widely applied to the fields such as paint, ink, plastics, ceramics, enamel.
Specific embodiment
The inventive method is described in detail below by way of specific embodiment.It is preferred that the purity of each raw material >=
99.99%.Calcination atmosphere must be oxidizing atmosphere, cause content to reduce to avoid cerium and tungsten from being reduced, and tinting strength, tinting power is reduced.Its
Middle carbamide does precipitant.
Embodiment 1
Weigh 32.3g cerous sulfates [Ce (SO under room temperature respectively4)2·4H2O], 7.1g Disulfatozirconic acid .s [Zr (SO4)2·4H2O], 66g tungsten
Sour sodium（Na2WO4·2H2O）Bottom liquid is configured in being added to the beaker equipped with 1L deionized waters, beaker is put in water bath and is risen
Temperature is stirred to being completely dissolved, is incubated 1h to 50 DEG C；Add 16.8g carbamide [CO (NH2)2], stir, use Dilute Ammonia Solution
（1mol/L）It is 9 to adjust pH value, is warming up to 90 DEG C, is incubated 2h.By product washing, sucking filtration, drying baker is put into, in 100 DEG C of temperature
Degree is lower to dry, and grinding is taken out after cooling, places in Muffle furnace with the ramp of 10 DEG C/min to 800 DEG C, and oxidizing atmosphere is protected
Warm 2h, crushes after natural cooling and obtains final product containing compound yellow material Ce of cerium0.8 Zr0.2 W2O8, L *=83.1, a ﹡=4.02, b *
= 69.1。
Use TiO2Carry out watering down test as diluent and show：Pigmenting power manufactured in the present embodiment can reach cadmium yellow
76.3%.
Embodiment 2
Weigh 36.3g cerous sulfates [Ce (SO under room temperature respectively4)2·4H2O], 2.4g titanium sulfates [Ti (SO4)2·9H2O], 66g tungsten
Sour sodium（Na2WO4·2H2O）Bottom liquid is configured in being added to the beaker equipped with 1L deionized waters, beaker is put in water bath and is risen
Temperature is stirred to being completely dissolved, is incubated 1h to 50 DEG C；Add 16.8g carbamide [CO (NH2)2], stir, use Dilute Ammonia Solution
（1mol/L）It is 9 to adjust pH value, is warming up to 90 DEG C, is incubated 2h.By product washing, sucking filtration, drying baker is put into, in 100 DEG C of temperature
Degree is lower to dry, and grinding is taken out after cooling, places in Muffle furnace with the ramp of 10 DEG C/min to 800 DEG C, and oxidizing atmosphere is protected
Warm 2h, crushes after natural cooling and obtains final product containing compound yellow material Ce of cerium0.9 Ti0.1W2O8, L *=79.3, a ﹡=5.63, b *=
66.3。
Use TiO2Carry out watering down test as diluent and show：Pigmenting power manufactured in the present embodiment can reach cadmium yellow
79.1%.
Embodiment 3
Weigh 32.3g cerous sulfates [Ce (SO under room temperature respectively4)2·4H2O], 3.6g Disulfatozirconic acid .s [Zr (SO4)2·4H2O], 2.4g sulfur
Sour titanium [Ti (SO4)2·9H2O], 66g sodium tungstates（Na2WO4·2H2O）It is configured in being added to the beaker equipped with 1L deionized waters
Bottom liquid, beaker is put in water bath and is warming up to 50 DEG C, is stirred to being completely dissolved, is incubated 1h；Add 16.8g carbamide [CO
(NH2)2], stir, use Dilute Ammonia Solution（1mol/L）It is 9 to adjust pH value, is warming up to 90 DEG C, is incubated 2h.By product water
Wash, sucking filtration, be put into drying baker, dry at a temperature of 100 DEG C, after cooling, take out grinding, place in Muffle furnace with 10 DEG C/
To 600 DEG C, oxidizing atmosphere insulation 2h is crushed after natural cooling and is obtained final product containing cerium compound yellow material Ce the ramp of min0.8
Zr0.1Ti0.1W2O8, L *=88.6, a ﹡=4.59, b *=67.2.
Use TiO2Carry out watering down test as diluent and show：Pigmenting power manufactured in the present embodiment can reach cadmium yellow
78.4%.
Embodiment 4
Weigh 26.0g cerous nitrates [Ce (NO under room temperature respectively3) 3·6H2O], 6.6g calcium nitrates [Ca (NO3)2], 65.2g potassium tungstates
(K2WO4) be added to the beaker equipped with 1L deionized waters in be configured to bottom liquid, beaker is put in water bath and is warming up to 50 DEG C, stirred
Mix to being completely dissolved, be incubated 1h；Add 16.8g carbamide [CO (NH2)2], stir, use Dilute Ammonia Solution（1mol/L）Adjust
Section pH value is 8, is warming up to 100 DEG C, is incubated 2h.By product washing, sucking filtration, drying baker is put into, is dried at a temperature of 100 DEG C,
Grinding is taken out after cooling, is placed in Muffle furnace with the ramp of 10 DEG C/min to 400 DEG C, oxidizing atmosphere insulation 2h is natural
Crush after cooling and obtain final product containing compound yellow material Ce of cerium0.6 Ca0.4 W2O8, L ﹡=84.9, a ﹡=0.81, b *=62.7.
Use TiO2Carry out watering down test as diluent and show：Pigmenting power manufactured in the present embodiment can reach cadmium yellow
82.3%.
Embodiment 5
Weigh 34.7g cerous nitrates [Ce (NO under room temperature respectively3)3·6H2O], 9.7g bismuth nitrate [Bi (NO3)3], 65.2g potassium tungstates
(K2WO4) be added to the beaker equipped with 1L deionized waters in be configured to bottom liquid, beaker is put in water bath and is warming up to 50 DEG C, stirred
Mix to being completely dissolved, be incubated 1h；Add 16.8g carbamide [CO (NH2)2], stir, use Dilute Ammonia Solution（1mol/L）Adjust
Section pH value is 10, is warming up to 70 DEG C, is incubated 2h.By product washing, sucking filtration, drying baker is put into, is dried at a temperature of 100 DEG C,
Grinding is taken out after cooling, is placed in Muffle furnace with the ramp of 10 DEG C/min to 1000 DEG C, oxidizing atmosphere insulation 2h is natural
Crush after cooling and obtain final product containing compound yellow material Ce of cerium0.8 Bi 0.2W2O8, L ﹡=89.7, a ﹡=0.32, b *=57.6.
Use TiO2Carry out watering down test as diluent and show：Pigmenting power manufactured in the present embodiment can reach cadmium yellow
74.9%.
Claims (10)
1. a kind of cerium Huang composite functional material, it is characterised in that molecular formula is Ce1-xMxW2O8, the M in formula be titanium, zirconium, calcium, bismuth its
In one or more, 0<x<1.
2. cerium according to claim 1 Huang composite functional material, it is characterised in that：0.1≤x≤0.4.
3. described in a kind of claim 1 or 2 cerium Huang composite functional material preparation method, it is characterised in that：By cerium salt, tungstates
With the salt of one or more in titanium, zirconium, calcium, bismuth in the presence of carbamide liquid phase synthesis, then by liquid phase synthesis product oxidation
400～1000 DEG C of calcinings in atmosphere.
4. the preparation method of cerium according to claim 3 Huang composite functional material, it is characterised in that：Titanium, zirconium, calcium or bismuth
Salt includes one or more in nitrate, sulfate, acetate and chloride, and cerium salt includes nitrate, sulfate and chlorination
One or more in thing, tungstates include one or more in alkali tungstates.
5. the preparation method of the yellow composite functional material of cerium according to claim 3 or 4, it is characterised in that：Carbamide and cerium salt
Mol ratio 3 ~ 4:1.
6. the preparation method of cerium according to claim 3 Huang composite functional material, it is characterised in that：Liquid phase synthesis pH=8～
10。
7. the preparation method of the yellow composite functional material of cerium according to claim 3 or 6, it is characterised in that：Liquid phase synthesis temperature
70～100 DEG C of degree.
8. the preparation method of the yellow composite functional material of cerium according to claim 3 or 6, it is characterised in that：During liquid phase synthesis
Between 1～3h.
9. the preparation method of cerium according to claim 3 Huang composite functional material, it is characterised in that：2～4h of calcination time.
10. the preparation method of the yellow composite functional material of cerium according to claim 3 or 6, it is characterised in that：Liquid phase synthesis are tied
Product is first washed and the drying in 100～300 DEG C of oxidizing atmosphere by beam.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3168410A (en) * | 1962-01-17 | 1965-02-02 | Harshaw Chem Corp | Praseodymium-cerium yellow |
| JP2006232601A (en) * | 2005-02-24 | 2006-09-07 | Osaka Univ | Yellow pigment |
| CN101186500A (en) * | 2007-12-11 | 2008-05-28 | 北京科技大学 | Cerium doping zirconium tungstate negative heat expansion conductive ceramic powder and preparation method thereof |
| CN101815675A (en) * | 2007-10-03 | 2010-08-25 | 日产化学工业株式会社 | Metal oxide composite sol, coating composition, and optical member |
| CN102634237A (en) * | 2012-03-30 | 2012-08-15 | 内蒙古大学 | Preparation method of novel composite pigment gamma-Ce2S3/SiO2 |
| CN103013185A (en) * | 2011-09-23 | 2013-04-03 | 北京大学 | Inorganic yellow pigment and preparation method thereof |
| CN105542516A (en) * | 2015-12-07 | 2016-05-04 | 陕西理工学院 | Yellow pigment able to reflect near infrared rays and preparation method thereof |
-
2016
- 2016-12-09 CN CN201611128943.8A patent/CN106590032A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3168410A (en) * | 1962-01-17 | 1965-02-02 | Harshaw Chem Corp | Praseodymium-cerium yellow |
| JP2006232601A (en) * | 2005-02-24 | 2006-09-07 | Osaka Univ | Yellow pigment |
| CN101815675A (en) * | 2007-10-03 | 2010-08-25 | 日产化学工业株式会社 | Metal oxide composite sol, coating composition, and optical member |
| CN101186500A (en) * | 2007-12-11 | 2008-05-28 | 北京科技大学 | Cerium doping zirconium tungstate negative heat expansion conductive ceramic powder and preparation method thereof |
| CN103013185A (en) * | 2011-09-23 | 2013-04-03 | 北京大学 | Inorganic yellow pigment and preparation method thereof |
| CN102634237A (en) * | 2012-03-30 | 2012-08-15 | 内蒙古大学 | Preparation method of novel composite pigment gamma-Ce2S3/SiO2 |
| CN105542516A (en) * | 2015-12-07 | 2016-05-04 | 陕西理工学院 | Yellow pigment able to reflect near infrared rays and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| SHINYA FURUKAWA等: "Synthesis of new environment-friendly yellow pigments", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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