CN101225244A - Sheet-like neodymium oxide and method for manufacturing same - Google Patents
Sheet-like neodymium oxide and method for manufacturing same Download PDFInfo
- Publication number
- CN101225244A CN101225244A CNA2008100036864A CN200810003686A CN101225244A CN 101225244 A CN101225244 A CN 101225244A CN A2008100036864 A CNA2008100036864 A CN A2008100036864A CN 200810003686 A CN200810003686 A CN 200810003686A CN 101225244 A CN101225244 A CN 101225244A
- Authority
- CN
- China
- Prior art keywords
- neodymium
- aqueous solution
- salt
- sheet
- suspensoid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Paper (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to a flake-shape neodymia and the manufacture method, which is characterized in that: in the flake-shape neodymia, the content of neodymia is 84.85wt% to 100wt%, and the content of alumina is 0 to 23.25wt%, and the content of silicon dioxide is 0 to 15.15wt%; the particle size is 10 Mum to 50 Mu m, and the thickness is less than 1 Mum; the manufacture method is that a water solution with neodymium salt and aluminum salt and a water solution with precipitator are prepared, and a plurality of mineralizer and phosphorous compound are dissolved in either water solution and then mixed to obtain a floating body or gel, and the floating body or gel is then vaporized and dried, and the production after drying is heated at 850 to 1450 degree centigrade with a molten salt process, and then a flake-shape neodymia is obtained. The flake-shape neodymia has the advantages of proper width to length ratio, smooth surface, high covering power, presenting different colors at different light sources, being widely used in plastic, coating, ink, cosmetic, glaze and anti-counterfeit and also being used as a base material of pearlescent pigment.
Description
Affiliated technical field
The present invention relates to a kind of is camouflage paint and preparation method, especially sheet-like neodymium oxide and the manufacture method thereof of main raw material with the Neodymium trioxide.
Background technology
Known a kind of neodymium pigment is arranged is by Neodymium trioxide and aluminum oxide, adds a small amount of mineralizer and stablizer in high-temperature calcination and synthetic.Above-mentioned Neodymium trioxide is a particulate state, and fraction of coverage is low.
Summary of the invention
For overcoming above-mentioned deficiency, the invention provides a kind of sheet-like neodymium oxide and manufacture method thereof.
The technical solution adopted for the present invention to solve the technical problems is:
First aspect relates to sheet-like neodymium oxide: Neodymium trioxide content is 84.85wt%-100wt% in the sheet-like neodymium oxide, and alumina content is 0-23.25wt%, and the content of silicon-dioxide is 0-15.15wt%; Described Neodymium trioxide median size is 10 μ m-50 μ m, and thickness is less than 1 μ m, aspect ratio, and promptly particle diameter/thickness is than greater than 20 laminar particle; Described Neodymium trioxide presents distinct colors under the Different Light irradiation.
Second aspect relates to the manufacture method of salic sheet-like neodymium oxide, this method may further comprise the steps: prepare the aqueous solution (i) of a kind of water-soluble neodymium salt and aluminium salt and a kind of aqueous precipitation agent aqueous solution (ii), the amount of substance of above-mentioned two kinds of aqueous solution solutes is suitable, at the aqueous solution (i) and the precipitation agent aqueous solution any uniform dissolution mineralizer and phosphorus compound in (ii), the mixed aqueous solution (i) and the precipitation agent aqueous solution (ii) obtain a kind of suspensoid or gel that contains reaction product, by this suspensoid of evaporation drying or gel, and heating comes fused salt to handle dried product under 850-1450 ℃, thereby obtain a kind of solid product, again it is washed, filter and drying.
The third aspect relates to the manufacture method of silica containing sheet-like neodymium oxide, this method may further comprise the steps: the aqueous solution for preparing a kind of water-soluble neodymium salt (iii) with a kind of alkalimetal silicate and precipitation agent aqueous solution mixing solutions (ii) (iv), mixing solutions (iv) the amount of substance of solute roughly the amount of substance with the water-soluble neodymium salt of the aqueous solution in (iii) is suitable, the aqueous solution (iii) with mixing solutions any in (iv) in uniform dissolution mineralizer and phosphorus compound, mixed aqueous solution (iii) (iv) obtains a kind of suspensoid or gel that contains reaction product with mixing solutions, by this suspensoid of evaporation drying or gel, and heating comes fused salt to handle dried product under 850-1450 ℃, thereby obtain a kind of solid product, again it is washed, filter and drying.
Fourth aspect relates to the manufacture method of the sheet-like neodymium oxide of oxygen-free aluminium and silicon-dioxide, this method may further comprise the steps: drip the solution of water-soluble neodymium salt and the precipitation agent aqueous solution simultaneously (ii) in water, make that the amount of substance of solute of the former with the latter is suitable, form suspensoid thus, in the aqueous solution of mineralizer, add this suspensoid, and in gained solution, add the solution of phosphorus compound, obtain the suspensoid or the gel of Heshui hydrolysis products, by this suspensoid of evaporation drying or gel, handle desciccate at 850-1450 ℃ of following fused salt and obtain a kind of solid product, again it is washed, filter and drying.
And:
Described Neodymium trioxide is pink colour under incandescent light, is blue under luminescent lamp, is red-purple under natural light.
Described aluminium salt is for being selected from aluminum chloride, Tai-Ace S 150, potassium aluminium sulfate, a kind of in the aluminum nitrate.
Described mineralizer is to be selected from a kind of in alkali metal chloride, the vitriol.
The described precipitation agent aqueous solution (ii) is the aqueous solution a kind of in alkali, alkaline carbonate, the oxalate.
Described phosphorus compound is selected from a kind of in phosphoric acid, the phosphoric acid salt.
The invention has the beneficial effects as follows: with the sheet-like neodymium oxide of method production provided by the invention, be difficult for forming twin and crystal reunion, particle is even more, the surface is Paint Gloss, and thickness is little, and aspect ratio (particle diameter/thickness) height has different color changeable effects under Different Light, is pink colour under incandescent light, being blue under luminescent lamp, is red-purple under natural light.Present method is simple, is easy to control and operation.
The present invention is further described below in conjunction with embodiment.
Embodiment 1:
The aqueous solution for preparing the aqueous solution (i) of a kind of water-soluble neodymium salt and aluminium salt and a kind of alkali or alkaline carbonate or oxalate (ii), its amount roughly with the above-mentioned aqueous solution (i) in the water-soluble neodymium salt and the amount of aluminium salt suitable, alkali metal chloride or vitriol and phosphoric acid or phosphoric acid salt in the aqueous solution (i) or the aqueous solution any uniform dissolution in (ii), mix the above-mentioned aqueous solution (i) and (ii) obtain a kind of suspensoid or gel that contains reaction product, by this suspensoid of evaporation drying or gel, and heating comes fused salt to handle dried product under 850-1450 ℃, thereby obtain a kind of solid product, again it is washed, filter and drying.
This method is by preparing two kinds of aqueous solution (i) and (ii) beginning.The aqueous solution (i) is made by water-soluble neodymium salt and aluminium salt.The former can be selected from various solubility neodymium salt, and wherein Neodymium trichloride is preferred, because they are easy to obtain and use and the difficult double salt precipitation that generates.Aluminium salt can be selected from aluminum chloride, Tai-Ace S 150, potassium aluminium sulfate, aluminum nitrate, wherein preferred aluminum chloride.The amount of aluminium salt requires with the shape (particle diameter, thickness, aspect ratio) of requirement product and variable color and changes.It accounts between the 0-23.25wt% of sheet Neodymium trioxide (salic) total amount (in oxide compound) usually.Aluminium salt is the principal element of mixing the variable color of aluminium flake shape Neodymium trioxide.
When preparation solution (i), heating can help the dissolving of each component.
The aqueous solution is (ii) made by alkali or alkaline carbonate or oxalate, its amount approximately with neutralization and hydrolysis water solution (i) in neodymium salt suitable with the required chemical equivalent of aluminium salt.Preferred alkali is sodium hydroxide and potassium hydroxide, and alkaline carbonate is yellow soda ash and salt of wormwood, and the preferred as alkali oxalate is sodium oxalate and potassium oxalate.
Add alkali metal chloride or vitriol (as mineralizer) and phosphoric acid or phosphoric acid salt (phosphorus compound) to the aqueous solution (i) or (ii).Two components can be added together (i) or (ii) in, also can be respectively with their add (i) and (ii) in.Importantly to guarantee them at solution (i) or the dissolving fully (ii), not produce double salt precipitation simultaneously.
The example of alkali metal chloride or vitriol (making mineralizer) comprises sodium-chlor, Repone K, and lithium chloride, sodium sulfate, vitriolate of tartar, and Lithium Sulphate, sodium-chlor wherein, Repone K are preferred, because they are easy to obtain, are difficult to produce the double salt precipitation of neodymium simultaneously.They also can use altogether.The amount of mineralizer (mole) should be water-soluble neodymium salt amount 2-6 doubly.When its amount is less than above-mentioned scope, mineralizer can not reach fused salt thermal treatment fully and form the effect of thin slice.And its amount is during more than above-mentioned scope, and mineralizer will cause wave useless, and can other effect not arranged to flakiness, and remove at the big water gaging of a subsequent step needs.
Phosphorus compound can be any phosphoric acid that is selected from, soluble phosphate, condensed phosphoric acid and solubility condensed phosphate.The example comprises phosphoric acid, Sodium phosphate dibasic, SODIUM PHOSPHATE, MONOBASIC, sodium phosphate, trisodium phosphate, tripoly phosphate sodium STPP, dipotassium hydrogen phosphate, potassium primary phosphate, potassium pyrophosphate, Potassium tripolyphosphate, and Secondary ammonium phosphate, primary ammonium phosphate, ammonium phosphate, tripolyphosphate ammonium.Phosphorus compound makes crystal make nucleator during the heating fused salt is handled and uses, and helps the crystal formation thin slice of Neodymium trioxide.When it measures less than 0.15wt%, can not make required sheet-like neodymium oxide.When it measures greater than 2.0wt%, it can not produce the additional effect that reduces sheet Neodymium trioxide thickness.
(ii) the time, heating will promote the dissolving of each component at preparation solution.
By stirring, will and (ii) mix as the above-mentioned aqueous solution that makes (i), to react.Mixing can be finished by following mode (1) or (2).
(1) drips simultaneously.This method comprises drip simultaneously the aqueous solution (i) and (ii) in water, makes the former roughly suitable with the latter.
(2) the simple interpolation.This method comprises solution (i) added solution (ii), or conversely and stir.Products obtained therefrom is reacted suspensoid or gel.
By the mixed suspensoid or the gel of getting of method (1) or (2), it contains the aqua oxidation neodymium, neodymium carbonate or neodymium oxalate, and mineralizer, hydrated aluminum oxide, and phosphorus compound, they are dispersed in the water medium.Suspensoid or gel are then by dehydration by evaporation and dry.To be used for exsiccant and to add heat in order to save, preferably make the aqueous solution (i) and (ii) by solution is made near saturated least quantity.Another approach that reaches this purpose is before above-mentioned (1) or (2) method begin, and by adding hydrothermal solution (i) and (ii), concentrates salt thus.In any case, the aqueous solution (i) and (ii) should contain a certain amount of water is to guarantee dissolving fully.If one or both in two kinds of solution all contain not dissolved substance, then their mixing can cause incomplete reaction, causes product generation twin and gathering, thereby product flakiness shape not, and inhomogeneous.In other words, the aqueous solution (i) and (ii) should be uniform dissolution.Tuo Shui product is then 850-1450 ℃ of following thermal treatment fully.The product that obtains washes with water to remove sticking free cpds (mainly being alkali-soluble salt) thereon.The last product of dry washing again.By this way, obtained the aluminiferous sheet-like neodymium oxide of expectation with discoloration effect.
Embodiment 2:
Xiang Shuizhong drips the solution of water-soluble neodymium salt and the solution of alkali or alkaline carbonate or oxalate simultaneously, make the roughly chemical equivalent of the former with the latter, form the suspensoid of hydronium(ion) oxidation neodymium and neodymium carbonate or neodymium oxalate thus, the solid that in the aqueous solution of alkali metal sulfates, adds this suspensoid or leach again by this suspensoid, and in gained solution, add aluminium salt and phosphoric acid or phosphatic solution, obtain containing the suspensoid or the gel of hydrolysate, by this suspensoid of evaporation drying or gel, handle desciccate at 850-1450 ℃ of following fused salt and obtain a kind of solid product, again it is washed, filter and drying.
Neodymium hydroxide Neodymium trihydroxide that present method will make in advance or neodymium carbonate or neodymium oxalate are as raw material, and this neodymium hydroxide Neodymium trihydroxide or neodymium carbonate or neodymium oxalate are made by above-mentioned first method is raw materials used.Neodymium hydroxide Neodymium trihydroxide is preparation like this, promptly drips the solution of water-soluble neodymium salt and the solution of alkali or alkaline carbonate or oxalate simultaneously in water, and makes alkali or alkaline carbonate or basic metal oxalate roughly be equivalent to the amount of neodymium salt.The suspensoid that contains aqua oxidation neodymium or carbonate or oxalate that obtains (or by washing and filter by the isolated solid of suspensoid) is joined in the aqueous solution as the alkali metal chloride of mineralizer or alkali metal sulfates again.The amount of alkali metal chloride or alkali metal sulfates is preferably 2-6 times (in mole) of the amount of water-soluble neodymium salt.And in the solution that obtains, add aluminium salt and phosphoric acid salt.The amount of aluminium salt (in aluminum oxide) is preferably the 0-23.25wt% of the amount of gained sheet Neodymium trioxide.Phosphatic amount (in P2O5) is preferably the 0.15-2.0wt% of the amount of gained Neodymium trioxide.The suspensoid that obtains is dewatered fully by evaporation with the mode identical with above-mentioned first method.In dehydrating step, thermal hydrolysis does not partly take place in the neodymium salt of hydrolysis yet.Dehydrating prods carries out fused salt under 850-1450 ℃ handles.Wash the product that obtains then with water.To remove adhesion free cpds (mainly being alkali-soluble salt) thereon.Final drying has obtained the salic laminar variable color Neodymium trioxide of expectation by this way through the product of washing.
Embodiment 3:
Prepare a kind of water-soluble neodymium salt (iii) with the mixing solutions of a kind of alkalimetal silicate and alkali or alkaline carbonate or oxalate (iv), its amount roughly amount with the water-soluble neodymium salt of the above-mentioned aqueous solution in (iii) is suitable, at the aqueous solution uniform dissolution alkali metal chloride or vitriol and phosphoric acid salt (iii) or in the aqueous solution any in (iv), mix the above-mentioned aqueous solution and (iii) and (iv) obtain a kind of suspensoid or gel that contains reaction product, by this suspensoid of evaporation drying or gel, and heating comes fused salt to handle dried product under 850-1450 ℃, thereby obtain a kind of solid product, again it is washed, filter and drying.
This method (iii) and is (iv) begun by two kinds of aqueous solution of preparation.The aqueous solution is (iii) made by water-soluble neodymium salt.Can be selected from various solubility neodymium salt, wherein Neodymium trichloride is preferred, because they are easy to obtain and use and the difficult double salt precipitation that generates.(iii) the time, heating can help the dissolving of each component at preparation solution.
The aqueous solution is (iv) made by alkalimetal silicate and alkali or alkaline carbonate or oxalate, and its amount is approximately suitable with the required chemical equivalent of neutralization and the hydrolysis water solution neodymium salt in (iii).Preferred alkalimetal silicate is a water glass, and potassium silicate, and preferred bases is sodium hydroxide and potassium hydroxide, and preferred alkali metal carbonate is yellow soda ash and salt of wormwood, and the preferred as alkali oxalate is sodium oxalate and potassium oxalate.The amount of alkalimetal silicate requires with the shape (particle diameter, thickness, aspect ratio) of requirement product and variable color and changes.It accounts between the 0-15.15wt% of sheet Neodymium trioxide (containing silicon-dioxide) total amount (in oxide compound) usually.Silicone content is the principal element of doped silicon slice shape Neodymium trioxide variable color.
Add alkali metal chloride or vitriol (as mineralizer) and phosphorus compound (iii) or (iv) to the aqueous solution.Two components can be added (iii) together or (iv), also can respectively their be added (iii) and (iv).To guarantee that importantly they at solution (iii) or the dissolving fully (iv), do not produce double salt precipitation simultaneously.
The example of alkali metal chloride or vitriol (making mineralizer) comprises sodium-chlor, Repone K, and lithium chloride, sodium sulfate, vitriolate of tartar, and Lithium Sulphate, sodium-chlor wherein, Repone K are preferred, because they are easy to obtain, are difficult to produce the double salt precipitation of neodymium simultaneously.They also can use altogether.The amount of mineralizer (mole) should be water-soluble neodymium salt amount 2-6 doubly.When its amount is less than above-mentioned scope, mineralizer can not reach fused salt thermal treatment fully and form the effect of thin slice.And its amount is during more than above-mentioned scope, and mineralizer will cause wave useless, and can other effect not arranged to flakiness, and remove at the big water gaging of a subsequent step needs.
Phosphorus compound can be any phosphoric acid that is selected from, soluble phosphate, condensed phosphoric acid and solubility condensed phosphate.The example comprises phosphoric acid, Sodium phosphate dibasic, SODIUM PHOSPHATE, MONOBASIC, sodium phosphate, trisodium phosphate, tripoly phosphate sodium STPP, dipotassium hydrogen phosphate, potassium primary phosphate, potassium pyrophosphate, Potassium tripolyphosphate, and Secondary ammonium phosphate, primary ammonium phosphate, ammonium phosphate, tripolyphosphate ammonium.As if phosphorus compound makes crystal make nucleator during the heating fused salt is handled and uses, and it helps the crystal formation thin slice of Neodymium trioxide.When it measures less than 0.15wt%, can not make required sheet-like neodymium oxide.When it measures greater than 2.0wt%, it can not produce the additional effect that reduces sheet Neodymium trioxide thickness.
(iv) the time, heating will promote the dissolving of each component at preparation solution.
By stirring, will (iii) and (iv) mix as the above-mentioned aqueous solution that makes, to react.Mixing can be finished by following mode (3) or (4).
(3) drip simultaneously.This method comprises and drips simultaneously the aqueous solution (iii) and (iv) in water, makes the former roughly suitable with the latter.
(4) the simple interpolation.This method comprises solution (iii) added solution (iv), or conversely and stir.Products obtained therefrom is reacted suspensoid or gel.
By the mixed suspensoid or the gel of getting of method (3) or (4), it contains the aqua oxidation neodymium, the silicic acid neodymium, and neodymium carbonate or neodymium oxalate, hydrated SiO 2, mineralizer, and phosphorus compound, they are dispersed in the water medium.Suspensoid or gel are then by dehydration by evaporation and dry.To be used for exsiccant and to add heat in order to save, preferably make the aqueous solution (iii) with (iv) by solution is made near saturated least quantity.Another approach that reaches this purpose is before above-mentioned (3) or (4) method begin, and by adding hydrothermal solution (iii) and (iv), concentrates salt thus.In any case, the aqueous solution (iii) and (iv) should contain a certain amount of water, to guarantee dissolving fully.If one or both in two kinds of solution all contain not dissolved substance, then their mixing can cause incomplete reaction, causes product generation twin and gathering, thereby product flakiness shape not, and inhomogeneous.In other words, the aqueous solution should be uniform dissolution (iii) and (iv).Tuo Shui product is then 850-1450 ℃ of following thermal treatment fully.The product that obtains washes with water to remove sticking free cpds (mainly being alkali-soluble salt) thereon.The last product of dry washing again.By this way, obtained the siliceous sheet-like neodymium oxide of expectation with discoloration effect.
Embodiment 4:
Xiang Shuizhong drips the solution of water-soluble neodymium salt and the solution of alkali or alkaline carbonate or oxalate simultaneously, make the roughly chemical equivalent of the former with the latter, form the suspensoid of hydronium(ion) oxidation neodymium and neodymium carbonate or neodymium oxalate thus, in the aqueous solution of alkalimetal silicate, add hydrochloric acid or sulfuric acid or nitric acid or phosphoric acid again, obtain the hydrated SiO 2 gel, contain the suspensoid of neodymium more than in alkali metal chloride or sulfate liquor, adding simultaneously again and contain the gel of hydration silicon-dioxide or by above two kinds of solids that system leaches, and in gained solution, add phosphoric acid or phosphatic solution, obtain containing the suspensoid or the gel of hydrolysate, by this suspensoid of evaporation drying or gel, handle desciccate at 850-1450 ℃ of following fused salt and obtain a kind of solid product, again it is washed, filter and drying.
Neodymium hydroxide Neodymium trihydroxide that present method will make in advance or neodymium carbonate or neodymium oxalate and hydrated SiO 2 are as raw material, and this neodymium hydroxide Neodymium trihydroxide or neodymium carbonate or neodymium oxalate are by raw materials used the making of above-mentioned the third method.Neodymium hydroxide Neodymium trihydroxide or neodymium carbonate or neodymium oxalate are preparations like this, promptly drip the solution of water-soluble neodymium salt and the solution of alkali or alkaline carbonate or oxalate simultaneously in water, and make alkali or alkaline carbonate or basic metal oxalate roughly be equivalent to the amount of neodymium salt.Hydrated SiO 2 is preparation like this, promptly in water, drip the bronsted lowry acids and bases bronsted lowry metal silicate simultaneously, and make the amount of sour amount and alkalimetal silicate suitable, with the suspensoid that contains aqua oxidation neodymium or carbonate or oxalate that obtains (or by washing and filter) and hydrated SiO 2 (or by washing and filtration by the isolated solid of suspensoid), join again in the aqueous solution as the alkali metal chloride of mineralizer or alkali metal sulfates by the isolated solid of suspensoid.The amount of alkali metal chloride or alkali metal sulfates is preferably 2-6 times (in mole) of the amount of water-soluble neodymium salt.And in the solution that obtains, add phosphide.The amount (in silicon-dioxide) of hydrated SiO 2 is preferably the 0-15.15wt% of the amount of the siliceous sheet Neodymium trioxide of gained in more than reacting.Phosphatic amount (in P2O5) is preferably the 0.15-2.0wt% of the amount of gained Neodymium trioxide.
The suspensoid that obtains is dewatered fully by evaporation with the mode identical with above-mentioned the third method.In dehydrating step, thermal hydrolysis does not partly take place in the salt of hydrolysis yet.Dehydrating prods carries out fused salt under 850-1450 ℃ handles.Wash the product that obtains then with water.To remove adhesion free cpds (mainly being alkali-soluble salt) thereon.Final drying has obtained the silica containing laminar variable color Neodymium trioxide of expectation by this way through the product of washing.
In order to study its physicals, with the flake aluminum oxide sample of the present invention of the above preparation of scanning electron microscopic observation.Find its median size 5-60 μ m, its thickness is less than 1 μ m, and aspect ratio is greater than 20.Find that also it does not have twin and gathering yet, and in water, disperse easily.
This Neodymium trioxide sample disperses and stirs the back to produce the streamline that similar mica produces in water in the aqueous solution, provable thus it good dispersiveness is arranged.Streamline is by the stratiform candy strip that suspends in liquid and the reflection ray on the laminar particulate of mobile surface forms.
Aluminium or silicon contained in chemical analysis its contained aluminium of proof of sheet-like neodymium oxide or silicon and the raw material are roughly suitable, and it only contains the phosphorus of trace.Can infer that phosphorus compound used in the inventive method produces the effect that makes the Neodymium trioxide sheet, but it is separated from system finally and is removed.
Therefore, the sheet-like neodymium oxide of the present invention definition is made up of Neodymium trioxide (as principal constituent) and aluminum oxide or silicon-dioxide (as auxilliary composition).
Sheet-like neodymium oxide pigment according to the present invention can be used as the pigment of pottery, or as paint, plastics, printing ink, the pigment of makeup or glaze.According to the purposes difference, also can further handle to give its water tolerance, weathering resistance, chemical resistance, anti-fadedness or high dispersibility.
Embodiment 5:
By being heated to about 55 ℃, with 1mol Neodymium trichloride and 1.5mol sodium-chlor, 1.5mol Repone K be dissolved in 300ml go obtain solution (i) from Yu Shuizhong.
Dissolving 0.4mol tertiary sodium phosphate and 3mol sodium hydroxide in the 250ml deionized water.The solution that makes is called the aqueous solution (ii).
Under agitation condition, with uniform rate with the aqueous solution (i) with (ii) to join in the 200ml deionized water, and make solute in the solution (i) simultaneously roughly suitable with the solute of solution in (ii).Continue to stir 15 minutes.Evaporation gained solution is to drying regime.The gained solid heated 4 hours down at about 1000 ℃.Add entry in the product that heat treated is crossed with the dissolving soluble salt.Leach insoluble solid, wash with water again, final drying.Obtain required sheet-like neodymium oxide thus.
Detect the sheet-like neodymium oxide that obtains with x diffraction analysis instrument.The peak that has only Neodymium trioxide in the diffraction pattern.Result by electron microscope observation shows that the sheet-like neodymium oxide particle diameter is 10-20 μ m, and the about 0.1 μ m of thickness does not produce twin.Good dispersion in the aqueous solution.
The gained sheet-like neodymium oxide is observed pink under incandescent light, be pearl opal under luminescent lamp, is red-purple under natural light.
Embodiment 6:
By being heated above 60 ℃, with 0.5mol Neodymium trichloride and 0.5mol aluminum chloride, 0.5mol sodium-chlor and 1.5mol Repone K are dissolved in the deionized water of 300ml, and the solution that makes is called the aqueous solution (i).
Dissolving 0.15mol tertiary sodium phosphate and 3mol sodium hydroxide in the 250ml deionized water.The solution that makes is called the aqueous solution (ii).
Under agitation condition, the aqueous solution (i) evenly joined be heated to about 60 ℃ aqueous solution (ii) in.Continue to stir 15 minutes, two kinds of solution mixtures that obtain are a kind of thick throw outs.Evaporation gained throw out is to drying regime.The gained solid heated 4 hours down at about 1100 ℃.Add entry in the product that heat treated is crossed with the dissolving soluble salt.Leach insoluble solid, wash with water again, final drying.Obtain required sheet-like neodymium oxide thus.
Detect the flake aluminum oxide that obtains with x diffraction analysis instrument.The peak that has only NdAlO3 in the diffraction pattern.Result by electron microscope observation shows that this sheet-like neodymium oxide particle diameter is 15-40 μ m, and the about 0.1 μ m of thickness does not produce twin.
When by dispersed with stirring in water the time, this sheet-like neodymium oxide has good dispersion.
The gained sheet-like neodymium oxide is observed pink under incandescent light, be blue under luminescent lamp, is purple under natural light.
Embodiment 7:
By being heated above 60 ℃, with the 1mol Neodymium trichloride, 0.5mol aluminum chloride and 1.5mol Repone K are dissolved in the deionized water of 300ml.Obtain solution (i).
Dissolving 0.4mol tertiary sodium phosphate and 4.5mol sodium hydroxide in the 250ml deionized water.Make the aqueous solution (ii).
Under agitation condition, with the aqueous solution (i) evenly adding be heated to about 60 ℃ aqueous solution (ii) in.Continue to stir 15 minutes.Two kinds of molten mixtures that obtain are a kind of thick precipitations.Evaporate this thick drying regime that is precipitated to.The gained solid heated 4 hours down at about 1100 ℃.Add water in the product after the heat treated with the dissolving soluble salt.Leach insoluble solid, wash with water again, final drying.Obtain required sheet-like neodymium oxide thus.
Detect the sheet-like neodymium oxide that obtains with x diffraction analysis instrument.The peak that Neodymium trioxide and aluminic acid neodymium are arranged in the diffraction pattern.Result by electron microscope observation shows that the flake aluminum oxide particle diameter is 15-40 μ m, and the about 0.1 μ m of thickness does not produce the contraction crystalline substance.
When by dispersed with stirring in water the time, this sheet-like neodymium oxide has good dispersion.
The gained sheet-like neodymium oxide is observed pink under incandescent light, be light blue under luminescent lamp, is red-purple under natural light.
Embodiment 8:
By being heated above 60 ℃, with the 1mol Neodymium trichloride, 2.5mol sodium-chlor and 1.5mol Repone K are dissolved in the deionized water of 300ml.Obtain solution (iii).
Dissolving 0.3mo tertiary sodium phosphate and 1.5mol water glass in the 250ml deionized water.The solution that makes is called the aqueous solution (iv).
Under agitation condition, with the aqueous solution (iv) join be heated to about 60 ℃ aqueous solution (iii) in.Continue to stir 15 minutes, the mixture of two kinds of solution of gained is a kind of thick precipitations.Evaporate this and be precipitated to drying regime.The gained solid heated 4 hours down at 1200 ℃.Add entry in the product after the heat treated so that the dissolving soluble salt.Leach insoluble solid, wash with water again, at last in dry.Obtain required sheet-like neodymium oxide thus.
Detect the sheet-like neodymium oxide that obtains with x diffraction analysis instrument.The peak that the silicic acid neodymium is arranged in the diffraction pattern.Result by electron microscope observation shows that the sheet-like neodymium oxide particle diameter is 20-50 μ m, and the about 0.2 μ m of thickness does not produce twin.When by dispersed with stirring in water the time, this sheet-like neodymium oxide has good dispersion.
The gained sheet-like neodymium oxide is observed pink under incandescent light, be light blue under luminescent lamp, is red-purple under natural light.
Embodiment 9:
By being heated above 60 ℃, with the 1mol Neodymium trichloride, 2.25mol sodium-chlor and 1.5mol Repone K be dissolved in 300ml go make the aqueous solution (iii) from Yu Shuizhong.
Dissolving 0.3mol tertiary sodium phosphate and 0.75mol water glass and 2.25mol sodium hydroxide in the 250ml deionized water.The solution that makes is called the aqueous solution (iv).
Under agitation condition, with the aqueous solution (iv) join be heated to about 60 ℃ aqueous solution (iii) in.Continue to stir 15 minutes, the mixture of two kinds of solution that obtain is a kind of thick precipitations.Evaporate this thick drying regime that is precipitated to.The gained solid heated 4 hours down at 1100 ℃.Add water in the product after the heat treated so that the dissolving soluble salt.Leach insoluble solid, wash with water again, final drying.Obtain required sheet-like neodymium oxide thus.
Detect the sheet-like neodymium oxide that obtains with x diffraction analysis instrument.The peak that Neodymium trioxide and silicic acid neodymium are arranged in the diffraction pattern.Result by electron microscope observation shows that the sheet-like neodymium oxide particle diameter is 15-30 μ m, and the about 0.2 μ m of thickness does not produce twin.
When by dispersed with stirring in water the time, sheet-like neodymium oxide has good dispersiveness.
The gained sheet-like neodymium oxide is observed pink under incandescent light, be light blue under luminescent lamp, is red-purple under natural light.
Claims (9)
1. sheet-like neodymium oxide, the Neodymium trioxide content that it is characterized in that it is 84.85wt%-100wt%, and alumina content is 0-23.25wt%, and the content of silicon-dioxide is 0-15.15wt%; Described Neodymium trioxide median size is 10 μ m-50 μ m, and thickness is less than 1 μ m, aspect ratio, and promptly particle diameter/thickness is than greater than 20 laminar particle; Described Neodymium trioxide presents distinct colors under the Different Light irradiation.
2. the manufacture method of a sheet-like neodymium oxide, it is characterized in that may further comprise the steps: prepare the aqueous solution (i) of a kind of water-soluble neodymium salt and aluminium salt and a kind of aqueous precipitation agent aqueous solution (ii), the amount of substance of above-mentioned two kinds of aqueous solution solutes is suitable, at the aqueous solution (i) and the precipitation agent aqueous solution any uniform dissolution mineralizer and phosphorus compound in (ii), the mixed aqueous solution (i) and the precipitation agent aqueous solution (ii) obtain a kind of suspensoid or gel that contains reaction product, by this suspensoid of evaporation drying or gel, and heating comes fused salt to handle dried product under 850-1450 ℃, thereby obtain a kind of solid product, again it is washed, filter and drying.
3. the manufacture method of a sheet-like neodymium oxide, it is characterized in that may further comprise the steps: the aqueous solution for preparing a kind of water-soluble neodymium salt (iii) with a kind of alkalimetal silicate and aqueous precipitation agent aqueous solution mixing solutions (ii) (iv), mixing solutions (iv) the amount of substance of solute roughly the amount of substance with the water-soluble neodymium salt of the aqueous solution in (iii) is suitable, the aqueous solution (iii) with mixing solutions any in (iv) in uniform dissolution mineralizer and phosphorus compound, mixed aqueous solution (iii) (iv) obtains a kind of suspensoid or gel that contains reaction product with mixing solutions, by this suspensoid of evaporation drying or gel, and heating comes fused salt to handle dried product under 850-1450 ℃, thereby obtain a kind of solid product, again it is washed, filter and drying.
4. the manufacture method of a sheet-like neodymium oxide, it is characterized in that may further comprise the steps: in water, drip the solution of water-soluble neodymium salt and the aqueous precipitation agent aqueous solution simultaneously (ii), make that the amount of substance of solute of the former with the latter is suitable, form suspensoid thus, in the aqueous solution of mineralizer, add this suspensoid, and in gained solution, add the solution of phosphorus compound, obtain the suspensoid or the gel of Heshui hydrolysis products, by this suspensoid of evaporation drying or gel, handle desciccate at 850-1450 ℃ of following fused salt and obtain a kind of solid product, again it is washed, filter and drying.
5. sheet-like neodymium oxide according to claim 1 is characterized in that: described Neodymium trioxide is pink colour under incandescent light, is blue under luminescent lamp, is red-purple under natural light.
6. the manufacture method of sheet-like neodymium oxide according to claim 2 is characterized in that: described aluminium salt is for being selected from aluminum chloride, Tai-Ace S 150, potassium aluminium sulfate, a kind of in the aluminum nitrate.
7. according to the manufacture method of claim 2 or 3 or 4 described sheet-like neodymium oxides, it is characterized in that: described mineralizer is to be selected from a kind of in alkali metal chloride, the vitriol.
8. according to the manufacture method of claim 2 or 3 or 4 described sheet-like neodymium oxides, it is characterized in that: the described precipitation agent aqueous solution (ii) is a kind of aqueous solution in alkali, alkaline carbonate, the oxalate.
9. according to the manufacture method of claim 2 or 3 or 4 described sheet-like neodymium oxides, it is characterized in that: described phosphorus compound is selected from a kind of in phosphoric acid, the phosphoric acid salt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100036864A CN101225244A (en) | 2008-01-11 | 2008-01-11 | Sheet-like neodymium oxide and method for manufacturing same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100036864A CN101225244A (en) | 2008-01-11 | 2008-01-11 | Sheet-like neodymium oxide and method for manufacturing same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101225244A true CN101225244A (en) | 2008-07-23 |
Family
ID=39857457
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008100036864A Pending CN101225244A (en) | 2008-01-11 | 2008-01-11 | Sheet-like neodymium oxide and method for manufacturing same |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101225244A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011242A (en) * | 2012-12-31 | 2013-04-03 | 江西理工大学 | Flaky lanthanum compound and preparation method thereof |
| CN103011241A (en) * | 2012-12-31 | 2013-04-03 | 江西理工大学 | Rare-earth praseodymium lamellar crystal and preparation method for same |
| CN114350350A (en) * | 2022-01-10 | 2022-04-15 | 华南理工大学 | Pigment with photoluminescence, mechanoluminescence and light-dependent heterochromatic effect as well as preparation method and application thereof |
-
2008
- 2008-01-11 CN CNA2008100036864A patent/CN101225244A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011242A (en) * | 2012-12-31 | 2013-04-03 | 江西理工大学 | Flaky lanthanum compound and preparation method thereof |
| CN103011241A (en) * | 2012-12-31 | 2013-04-03 | 江西理工大学 | Rare-earth praseodymium lamellar crystal and preparation method for same |
| CN103011242B (en) * | 2012-12-31 | 2015-03-18 | 江西理工大学 | Flaky lanthanum compound and preparation method thereof |
| CN103011241B (en) * | 2012-12-31 | 2015-03-18 | 江西理工大学 | Rare-earth praseodymium lamellar crystal and preparation method for same |
| CN114350350A (en) * | 2022-01-10 | 2022-04-15 | 华南理工大学 | Pigment with photoluminescence, mechanoluminescence and light-dependent heterochromatic effect as well as preparation method and application thereof |
| CN114350350B (en) * | 2022-01-10 | 2023-02-14 | 华南理工大学 | Pigment with photoluminescence, mechanoluminescence and light-dependent heterochromatic effect as well as preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101824236B (en) | Preparation process of medium temperature resistant iron oxide black | |
| CN102515853B (en) | Preparation method of zirconium silicate wrapped high-temperature sulfur cadmium selenide bright red pigment | |
| CN111017934B (en) | Bioactive silicon regenerative medical material and preparation method thereof | |
| CN101225244A (en) | Sheet-like neodymium oxide and method for manufacturing same | |
| CN104371717A (en) | Preparation method for enhancing luminescence property of BiPO4:Eu fluorescent powder by shape regulation | |
| CN102241528B (en) | Process for preparing spherical nanometer spinel zaffre by hydrothermal method | |
| CN107473707A (en) | A kind of crowded mud method luminescent ceramic pug composition and preparation method thereof | |
| CN103011242B (en) | Flaky lanthanum compound and preparation method thereof | |
| CN103011241B (en) | Rare-earth praseodymium lamellar crystal and preparation method for same | |
| CN113479895A (en) | Method for preparing superfine zirconium silicate and zirconium silicate-based coating pigment by one-step precipitation method | |
| CN110182818B (en) | Calcium-chromium garnet green pigment and preparation method thereof | |
| CN109705621B (en) | Superfine silicon dioxide coated bismuth molybdate-vanadate yellow pigment and preparation method thereof | |
| CN106590031A (en) | Cadmium sulfoselenide occlusion pigment, ceramic ink and preparation method of cadmium sulfoselenide occlusion pigment | |
| CN114620698B (en) | Large-particle zirconium phosphate and preparation method thereof | |
| CN107815142B (en) | Nano vanadium-zirconium blue ceramic pigment and preparation method thereof | |
| CN104710192A (en) | Zirconium phosphate high-temperature nickel red ceramic pigment and preparation method thereof | |
| CN102060570B (en) | High-temperature underglaze gold ruby pigment and preparation method thereof | |
| CN107033656A (en) | A kind of heat resistant type ferric oxide yellow pigment and preparation method thereof | |
| CN109338454A (en) | The preparation method of the siliceous titanium dioxide crystal whisker of rutile-type | |
| CN101239741A (en) | Preparation method for nanometer chrome oxide particle | |
| CN105925014A (en) | Ferric oxide yellow pigment and preparation method thereof | |
| CN101148258B (en) | Method for preparing hydrated aluminum silicate | |
| CN100395178C (en) | Method of producing zinc phosphate using phosphorus fertilizer | |
| CN102220038A (en) | [Alpha]-alumina single-crystal slices, and preparation method thereof | |
| JP3711318B2 (en) | Method for producing alumina particles |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20080723 |