CN100523095C - Low infrared emittance sheet-like pigment and method for preparing same - Google Patents
Low infrared emittance sheet-like pigment and method for preparing same Download PDFInfo
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- CN100523095C CN100523095C CNB200510027124XA CN200510027124A CN100523095C CN 100523095 C CN100523095 C CN 100523095C CN B200510027124X A CNB200510027124X A CN B200510027124XA CN 200510027124 A CN200510027124 A CN 200510027124A CN 100523095 C CN100523095 C CN 100523095C
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- pigment
- aqueous solution
- flake aluminum
- iron salt
- divalent iron
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Abstract
The invention discloses the aluminum dust dye and preparing method. The dye has emissing ability, and is covered with ferrite yellow. The particle mean size of aluminum dust is 1-100 mum, and the aluminum dust is lack-lustre, golden ocher, and good oxidation resistance. The average emissing ability of infrared band is 0.50-0.60.
Description
Technical field
The present invention relates to a kind of low infrared emittance sheet-like pigment and preparation method thereof, relate in particular to a kind of by flake aluminum and the coat composed pigment of a hydrated ferric oxide that is wrapped in outside it.
Background technology
Infrared stealth technology is at means such as infrared imaging, infrared guidance and infrared reconnaissances and the infrared target control techniques that grows up.
The infrared stealth material is a military material of hi-tech that emerges the middle and later periods in 20th century, makes infrared stealth coating or the stealthy shield of infrared camouflage color with different infrared emittances with it, can realize stealthy for military target.
Optical research shows that the reflectivity of opaque article is high more, and emittance is just low more, and therefore the metal of high reflectance being arranged is most important pigment type in the infrared stealth coating.In fact most widely used is excellent property, cheap metallic aluminium powder.The particle shape of metallic pigment, size have remarkably influenced to the infrared emittance of coating, and size is lower with other form aluminium powder emittance than spherical in its infrared emittance of flaky aluminum of 10～100 μ m, and effect is best.
In the last century eighties, the several military powers in west are all without exception adds a large amount of aluminium foils in infrared stealth coating, to reduce infrared emittance and to be used for military equipment in a large number.But because the adding of aluminium flake makes coating strengthen visible reflection of light, be difficult to merge, be unfavorable for that visible light is stealthy with background; The oxidation-resistance of aluminium flake is relatively poor simultaneously, and long-term exposure is oxidation easily in air, and emittance increases greatly after the oxidation, and the existence of these unfavorable factors is very limited metallic aluminium powder in actual applications.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of low infrared emittance sheet-like pigment and preparation method thereof, to overcome the above-mentioned defective that prior art exists, satisfy the needs of military material field development.
Low infrared emittance sheet-like pigment of the present invention is made up of flake aluminum and hydrated ferric oxide coating that is wrapped in outside it, and wherein the mass ratio of the quality of a hydrated ferric oxide and flake aluminum is 1:2～2:1.
The chemical structural formula of a said hydrated ferric oxide is:
Fe
2O
3H
2O or FeOOH
Its diameter of said low infrared emittance sheet-like pigment is 10 microns～100 microns, radius-thickness ratio: 60～80.
The preparation method of low infrared emittance sheet-like pigment of the present invention comprises the steps:
With the aqueous solution of divalent iron salt and flake aluminum under 25～50 ℃ temperature, add alkaline aqueous solution adjusting pH value and reach 3～4, beginning bubbling air, the oxidizing reaction of generation iron ion, constantly replenish alkaline aqueous solution simultaneously, the pH value of reaction solution is remained between 3～5; As ferrous ion (Fe
2+) concentration when reaching 0.001～0.003mol/L, regulate pH=6.0～6.7, stop blowing air, adopt conventional method from reaction product, to collect the flake aluminum pigment of the fine and close ferric oxide of surface coating then.
Ferric oxide is a hydrous iron oxide in the sheet metal aluminium powder pigment of the fine and close ferric oxide of surface coating of the present invention, and following reaction takes place in the process of the synthetic hydrous iron oxide of ferrous iron inorganic salt:
Fe
2++2OH
-＝Fe(OH)
2↓ (1)
Fe(OH)
2+1/4O
2＝FeOOH+1/2H
2O (2)
Said divalent iron salt is selected from FeSO
4Or FeCl
2In a kind of mixture of or these two kinds of salt.FeSO
4Can adopt the by product green vitriol (FeSO in the sulfuric acid method titanium pigment production process
47H
2O) or other technical grade commercially available prod.Iron protochloride can adopt the byproduct FeCl that produces in the pickled plate process
2Solution or commercially available moisture salt also can adopt well-known hydrochloric acid to steep the method on-site preparation of iron sheet.
The concentration of the aqueous solution of divalent iron salt is 0.01mol/L～0.30mol/L, preferably at 0.05mol/L～0.25mol/L.Lower ferrous iron concentration helps the heterogeneous nucleation of ferric oxide on the aluminium powder surface, avoids the homogeneous nucleation of ferric oxide.The homogeneous nucleation of ferric oxide will cause ferric oxide to descend at effective clad ratio on aluminium powder surface, finally influence the infrared emittance of product pigment.
The said flake aluminum of the present invention can adopt commercially available pigment-level aluminium powder, grinds through ball milled to obtain.Its length and width mean sizes are 10 μ m～100 μ m, radius-thickness ratio: 60～80.The solids concn of flake aluminum pigment in the divalent iron salt aqueous solution is 2g/L～100g/L, is preferably 8g/L～60g/L;
In the divalent iron salt aqueous solution, the mass ratio of divalent iron salt and flake aluminum is:
Divalent iron salt: flake aluminum=1:0.3～1:1 makes that the ratio of a hydrated ferric oxide quality and aluminium powder quality is 1:2～2:1 in the gained pigment products.
Said alkaline aqueous solution is selected from a kind of in aqueous sodium hydroxide solution, ammoniacal liquor or the aqueous sodium carbonate.The concentration of alkaline aqueous solution is pressed OH
-Volumetric molar concentration is counted 0.05mol/L～3mol/L, lower alkali concn helps the heterogeneous nucleation of ferric oxide and to effective coating on aluminium powder surface, adopting higher alkali concn is favourable to the economy of process, and therefore best alkali concn is 0.1mol/L～1.5mol/L.
Before adding alkaline aqueous solution, the temperature of reaction system should be controlled between 25～50 ℃, and adopts common stirring means mixing stirring.Crossing low temperature needs refrigated cooling, and too high temperature then can generate Fe
3O
4Deng impurity and can not obtain the satisfactory product of color.
The rate of addition of strict control alkaline aqueous solution and the feeding speed of air are come controls reaction speed in the reaction process, when speed of response arrives to a certain degree slowly, the ferric oxide that generates the just overwhelming majority is coated on the surface of aluminium flake, thereby obtains the aluminium flake of surperficial coated iron oxide.In order to reach this purpose, the feeding speed of air and the adding speed of alkaline aqueous solution should make the pH value of reaction system maintain between 3～5.
Ultimate principle of the present invention is: the surface at flake aluminum coats fine and close ferric oxide chemical coating, has solved the problem of oxidation of metallic aluminium powder surface metal aluminium on the one hand, on the other hand because surface oxidation iron has changed the metallicity gloss and the color of aluminium powder.The flake aluminum pigment of surperficial coated iron oxide of the present invention possesses following effect: emittance is low, satisfies the requirement of infrared stealth substantially; Color is a khaki color, is one of visible light camouflage color primitive colour, and the stealthy compatible basis of good multiband is arranged; Good in oxidation resistance was placed 24 hours down at 180 ℃, and its performance does not change.
Because the hydrated ferric oxide coating that is provided with of the present invention, the surface does not have metalluster, but has the suitable infrared low-emissivity of aluminium powder (under wavelength 8～14 μ m, emittance is 0.50～0.65), its diameter can be 10 microns～100 microns, can satisfy the requirement to pigment of infrared stealth coating or infrared camouflage painting.
Description of drawings
Fig. 1 is the electron scanning micrograph of making after the coating.
Embodiment
Embodiment 1
Take by weighing 13.9gFeSO
47H
2O with water dissolution and be diluted to 1L, takes by weighing 4gNaOH with water dissolution and be diluted to 500ml; With FeSO
4Solution is poured the 2L reactor into, drops into flake aluminum 20g then, stirs, and reactor heats with the hot water jacket; When temperature rose to 30 ℃ of design temperatures, adding volumetric molar concentration was the NaOH solution of 0.2mol/L, and the rate of addition with peristaltic pump control NaOH solution makes the pH value of reaction solution remain on 5; When the pH value reaches 3.5, use the air compressor machine bubbling air, air flow control is at 500ml/min; In the reaction process, every sampling in a hour once, measure Fe with the potassium bichromate standard solution titration
2+Concentration, work as Fe
2+Concentration during less than 0.003mol/L, regulate pH=6.0, stop bubbling air.Suction filtration, washing, 115 ℃ dry down, get final product the about 40g of flake aluminum of surperficial coating iron oxide yellow.
Color is a khaki color, matt, (test philosophy is seen document to the IR-1 type infrared emittance tester that adopts Shanghai Institute of Technical Physics of the Chinese Academy of Sciences to produce: Zhang Caigen, highly sensitive infrared thermometer is used for two gardens tube method and measures emissivity, infrared and millimeter wave journal, 1991,10 (5): 385) disclosed method detects, the average emitted rate of infrared band (wavelength 8～14 μ m) is 0.56, and the electron scanning micrograph of making after the coating is seen accompanying drawing 1.
Embodiment 2
Take by weighing 69.5gFeSO
47H
2O, with water dissolution and be diluted to 1L, compound concentration is that the ammonia soln 500ml of 1.0mol/L is standby; With FeSO
4Solution is poured the 2L reactor into, and dropping into median size then is the flake aluminum 30g of 40 μ m, stirs reactor thermostatic bath heating in water bath; When temperature rose to 50 ℃ of design temperatures, adding volumetric molar concentration was the ammonia soln of 1.0mol/L, and the rate of addition with peristaltic pump control ammonia soln makes the pH value of reaction solution remain on 4.5; When the pH value reaches 3.5, use the air compressor machine bubbling air, air flow control is at 500ml/min; In the reaction process, every sampling in a hour once, measure Fe with the potassium bichromate standard solution titration
2+Concentration, work as Fe
2+Concentration during less than 0.003mol/L, regulate pH=6.0, stop bubbling air.Suction filtration, washing, 100 ℃ dry down, get final product the about 60g of flake aluminum of surperficial coating iron oxide yellow.Color is a khaki color, tarnish, and the average emitted rate of infrared band (wavelength 8～14 μ m) is 0.58.
Embodiment 3
Take by weighing 20gFeCl
24H
2O with water dissolution and be diluted to 1L, takes by weighing 53gNa
2CO
3With water dissolution and be diluted to 500mL; With FeCl
2Solution is poured in the 2L reactor, and dropping into median size then is 20 μ m flake aluminum 20g, stirs reactor thermostatic bath heating in water bath; When temperature rises to 40 ℃ of design temperatures, add mass concentration and be 10.6% aqueous sodium carbonate, control Na with peristaltic pump
2CO
3The rate of addition of the aqueous solution makes the pH value of reaction solution remain on 4; When the pH of reaction solution value reaches 4, use the air compressor machine bubbling air, air flow control is at 500mL/min; In the reaction process, every sampling in a hour once, measure Fe with the potassium bichromate standard solution titration
2+Concentration, work as Fe
2+Concentration during less than 0.003mol/L, regulate pH=6, stop bubbling air.Suction filtration, washing, 150 ℃ down dry, get final product the about 40g of flake aluminum of surperficial coating iron oxide yellow.
Color is a khaki color, tarnish, and the average emitted rate of infrared band (wavelength 8～14 μ m) is about 0.6.
Claims (8)
1. a low infrared emittance sheet-like pigment is characterized in that, is made up of flake aluminum and hydrated ferric oxide coating that is wrapped in outside it, and wherein the mass ratio of the quality of a hydrated ferric oxide and flake aluminum is 1:2～2:1, and color is a khaki color.
2. low infrared emittance sheet-like pigment according to claim 1 is characterized in that, diameter is 10 microns～100 microns, radius-thickness ratio: 60～80.
3. the preparation method of low infrared emittance sheet-like pigment according to claim 1 and 2 is characterized in that, comprises the steps:
With the aqueous solution of divalent iron salt and flake aluminum under 25～50 ℃ temperature, add alkaline aqueous solution adjusting pH value and reach 3～4, beginning bubbling air, the oxidizing reaction of generation iron ion, constantly replenish alkaline aqueous solution simultaneously, the pH value of reaction solution is remained between 3～5; As ferrous ion (Fe
2+) concentration when reaching 0.001～0.003mol/L, regulate pH=6.0～6.7, stop blowing air, adopt conventional method from reaction product, to collect the flake aluminum pigment of the fine and close ferric oxide of surface coating then.
4. method according to claim 3 is characterized in that said divalent iron salt is selected from FeSO
4Or FeCl
2In a kind of mixture of or these two kinds of salt.
5. method according to claim 4 is characterized in that, the concentration of the aqueous solution of divalent iron salt is 0.01mol/L～0.30mol/L.
6. method according to claim 5 is characterized in that, said flake aluminum is of a size of 10 μ m～100 μ m.
7. method according to claim 3 is characterized in that, the solids concn of sheet metal aluminium powder pigment in the divalent iron salt aqueous solution is 2g/L～100g/L.
8. method according to claim 3 is characterized in that, in the divalent iron salt aqueous solution, the mass ratio of divalent iron salt and flake aluminum is:
Divalent iron salt: flake aluminum=1:0.3～1:1.
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|---|---|---|---|
| CNB200510027124XA CN100523095C (en) | 2005-06-24 | 2005-06-24 | Low infrared emittance sheet-like pigment and method for preparing same |
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|---|---|---|---|
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618157B (en) * | 2012-03-23 | 2014-04-09 | 电子科技大学 | Infrared low-emissivity coating material and preparation method thereof |
| CN103306131B (en) * | 2013-06-21 | 2016-01-20 | 中国人民解放军总后勤部军需装备研究所 | A kind of infrared low-emissivity khaki invisible coating and preparation method thereof |
| CN104629498B (en) * | 2015-02-04 | 2017-05-03 | 电子科技大学 | Magnetic low-infrared-radiation composite material and preparation method thereof |
| CN107163625B (en) * | 2017-06-09 | 2019-04-16 | 河北大学 | A kind of preparation method of the color aqueous aluminium powder pigment of ferriferous oxide cladding |
| CN108339988A (en) * | 2018-01-26 | 2018-07-31 | 华南理工大学 | A kind of plasmaassisted ball milling prepares method and the application of flake aluminum |
| CN115651443A (en) * | 2022-10-31 | 2023-01-31 | 中昊北方涂料工业研究设计院有限公司 | Low-infrared-emissivity functional filler compatible with visible light camouflage |
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Granted publication date: 20090805 Termination date: 20180624 |