Green-leaf-imitating spectrum rare earth pigment composition and preparation method thereof

Abstract

The invention discloses a green-leaf-imitating spectrum rare earth pigment composition and a preparation method thereof, the green-leaf-imitating spectrum rare earth pigment composition is prepared by mixing raw materials including chromic oxide, a rare earth compound, a spectrum regulator, a dispersing agent, a complexing agent, a pH regulator and deionized water, the rare earth compound is selected from rare earth oxide, rare earth chloride and rare earth nitrate, and the spectrum regulator is selected from a spectrum regulator and a dispersing agent. Wherein the rare earth elements are selected from gadolinium, praseodymium, europium, dysprosium, holmium and erbium. The invention has good green leaf spectrum imitating performance, and can provide an omnibearing camouflage effect covering a visible light wave band and a near-infrared wave band; the preparation method is simple, raw materials are easy to obtain, and the method is suitable for industrial production.

Description

Technical Field

[0001] The invention belongs to the technical field of rare earth compound application, and in particular relates to a green leaf-like spectrum rare earth pigment composition and a preparation method thereof. Background Art

[0002] Vegetation environment is one of the typical combat backgrounds for camouflaged targets. In order to improve the camouflage effect of personnel and equipment on the battlefield, especially the spectral camouflage against the background of plants, it is particularly important to study and invent optical camouflage materials with spectral characteristics that imitate green vegetation. In the natural environment, the spectral characteristics of vegetation are the result of its interaction with the surrounding environment. This characteristic exhibits unique reflection and absorption characteristics in the visible and near-infrared bands. Ideal optical camouflage materials should be able to imitate these characteristics to achieve a full range of camouflage effects. This requires that the camouflage material should not only show a color similar to that of vegetation in the visible light band, but also show a spectral reflectivity similar to that of vegetation in the near-infrared band.

[0003] Most existing green pigments use organic pigments such as copper phthalocyanine, which can indeed provide a certain camouflage effect in the visible light range. However, under near-infrared spectral reconnaissance, due to the large spectral difference, the camouflaged target is easily exposed, which highlights the urgency and importance of developing new optical camouflage materials. Summary of the invention

[0004] The present invention aims to overcome the defects of the prior art and provide a rare earth pigment composition imitating green leaf spectrum.

[0005] Another object of the present invention is to provide a method for preparing the above-mentioned green leaf-like spectrum rare earth pigment composition.

[0006] The technical solution of the present invention is as follows:

[0007] A green leaf-like spectrum rare earth pigment composition is prepared by mixing chromium oxide, a rare earth compound, a spectrum regulator, a dispersant, a complexing agent, a pH regulator and deionized water, wherein:

[0008] The rare earth compound is selected from rare earth oxide, rare earth chloride and rare earth nitrate, wherein the rare earth element is selected from gadolinium, praseodymium, europium, dysprosium, holmium and erbium.

[0009] In a preferred embodiment of the present invention, the rare earth element is selected from praseodymium, dysprosium, holmium and erbium.

[0010] Further preferably, the rare earth compound is selected from ErCl3·6H2O, DyCl3·6H2O, Er(NO3)3·6H2O, Ho(NO3)3·6H2O and PrCl3·6H2O.

[0011] In a preferred embodiment of the present invention, the spectrum modifier is selected from zinc oxide, cobalt oxide and nickel oxide.

[0012] In a preferred embodiment of the present invention, the dispersant is selected from polyvinyl pyrrolidone, polyvinyl alcohol, sodium dodecylbenzene sulfonate and polyethylene glycol.

[0013] In a preferred embodiment of the present invention, the complexing agent is selected from citric acid, ethylenediaminetetraacetic acid, pyrophosphoric acid, ethylenediamine and urea.

[0014] In a preferred embodiment of the present invention, the pH adjuster is selected from hydrochloric acid and nitric acid.

[0015] In a preferred embodiment of the present invention, the rare earth compound is PrCl3·6H2O, the spectrum regulator is nickel oxide, the dispersant is polyethylene glycol, the complexing agent is urea, and the pH regulator is nitric acid.

[0016] In a preferred embodiment of the present invention, the mass ratio of the chromium oxide, the rare earth compound, the spectrum modifier, the dispersant and the complexing agent is 100:60-100:5-10:1-5:30-100.

[0017] The method for preparing the above-mentioned green leaf-like spectrum rare earth pigment composition comprises the following steps:

[0018] (1) Dispersing Cr2O3 powder and spectrum modifier in deionized water, ultrasonicating for 10-60 min, then adding dispersant, stirring at 60-90°C for 30-90 min, filtering, and drying at 80-120°C for 4-12 h to obtain material A;

[0019] (2) dissolving the rare earth compound in deionized water, and then adding a pH adjuster to a pH of 1-3 to obtain material B;

[0020] (3) dispersing material A in a complexing agent, stirring at 100-150° C. for 30-90 min, to obtain material C;

[0021] (4) Material C is added dropwise to material B, stirred and refluxed at 100-150°C for 30-120 min, and then the precipitate is collected, washed with deionized water, and dried at 80-120°C for 4-12 h to obtain material D;

[0022] (5) Calcine material D at 600-1100°C for 1-3h to obtain.

[0023] The beneficial effects of the present invention are:

[0024] 1. The present invention has good green leaf imitation spectral performance and can provide a full range of camouflage effects covering the visible light band and near infrared band.

[0025] 2. The preparation method of the present invention is simple, the raw materials are readily available, and it is suitable for industrial production. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 The green leaf spectrum of the rare earth pigment composition E5 prepared in Example 5 of the present invention is compared with the green leaf spectrum.

[0027] Figure 2 This is the XRD diagram of the green leaf spectral rare earth pigment composition E5 prepared in Example 5 of the present invention.

[0028] Figure 3 This is a scanning electron microscope photograph of the green leaf-like spectral rare earth pigment composition E5 prepared in Example 5 of the present invention. DETAILED DESCRIPTION

[0029] The technical solution of the present invention is further illustrated and described below through specific implementation modes in combination with the accompanying drawings.

[0030] Example 1

[0031] (1) 100 parts by weight of Cr2O3 and 5 parts by weight of a spectrum modifier, zinc oxide, were dispersed in 500 parts by weight of deionized water, ultrasonicated for 10 minutes, and then 1 part by weight of a dispersant, polyvinyl pyrrolidone (PVP), was added, placed in a 60°C water bath, magnetically stirred for 30 minutes, filtered, and dried at 80°C for 12 hours to obtain A1;

[0032] (2) dissolving 60 parts by weight of ErCl3·6H2O in 500 parts by weight of deionized water, and then adding an appropriate amount of a pH adjuster-hydrochloric acid until the pH value of the final ErCl3 solution is 1, to obtain B1;

[0033] (3) A1 was dispersed in 30 parts by weight of a complexing agent, citric acid, and placed in an oil bath at 100° C. and magnetically stirred for 30 min to obtain C1;

[0034] (4) C1 was added dropwise to B1 at a rate of 0.5 mL / min, stirred and refluxed in an oil bath at 100°C for 30 min, and then the precipitate was collected by filtration using a Buchner funnel, rinsed three times with deionized water, and then dried in an oven at 80°C for 12 h to obtain D1;

[0035] (5) D1 was placed in a muffle furnace and calcined at 600°C for 3 h to obtain the rare earth bionic pigment E1.

[0036] Example 2

[0037] (1) 100 parts by weight of Cr2O3 and 8 parts by weight of a spectrum modifier, cobalt oxide, were dispersed in 500 parts by weight of deionized water, and ultrasonicated for 30 minutes. Then, 3 parts by weight of a dispersant, polyvinyl alcohol (PVA), were added, and the mixture was placed in a water bath at 80° C., magnetically stirred for 60 minutes, and then filtered and dried at 100° C. for 6 hours to obtain A2;

[0038] (2) dissolving 100 parts by weight of DyCl3·6H2O in 500 parts by weight of deionized water, and then adding an appropriate amount of a pH adjuster - hydrochloric acid until the pH value of the final DyCl3 solution is 2, to obtain B2;

[0039] (3) A2 was dispersed in 60 parts by weight of a complexing agent, ethylenediaminetetraacetic acid, placed in an oil bath at 120° C., and magnetically stirred for 60 min to obtain C2;

[0040] (4) C2 was added dropwise to B2 at a rate of 1 mL / min, stirred and refluxed in an oil bath at 120°C for 60 min, and then the precipitate was collected by filtration using a Buchner funnel, rinsed three times with deionized water, and then dried in an oven at 100°C for 6 h to obtain D2;

[0041] (5) D2 is placed in a muffle furnace and calcined at 700° C. for 3 h to obtain the green leaf spectrum rare earth pigment composition E2.

[0042] Example 3

[0043] (1) 100 parts by weight of Cr2O3 and 10 parts by weight of a spectrum modifier, nickel oxide, were dispersed in 500 parts by weight of deionized water, and ultrasonicated for 60 minutes. Then, 5 parts by weight of a dispersant, sodium dodecylbenzene sulfonate, were added, and the mixture was placed in a 90° C. water bath, magnetically stirred for 90 minutes, filtered, and dried at 120° C. for 4 hours to obtain A3;

[0044] (2) dissolving 600 parts by weight of Er(NO3)3·6H2O in 500 parts by weight of deionized water, and then adding an appropriate amount of pH adjuster-nitric acid until the final pH value of the Er(NO3)3 solution is 3, to obtain B3;

[0045] (3) A3 was dispersed in 100 parts by weight of a complexing agent, pyrophosphoric acid, placed in an oil bath at 150° C., and magnetically stirred for 90 min to obtain C3;

[0046] (4) C3 was added dropwise to B3 at a rate of 2 mL / min, and the mixture was stirred and refluxed in an oil bath at 150°C for 120 min. The precipitate was then collected by filtration using a Buchner funnel, rinsed three times with deionized water, and then dried in an oven at 120°C for 4 h to obtain D3.

[0047] (5) D3 was placed in a muffle furnace and calcined at 700° C. for 3 h to obtain the green leaf-like spectrum rare earth pigment composition E3.

[0048] Example 4

[0049] (1) 100 parts by weight of Cr2O3 and 6 parts by weight of a spectrum modifier, nickel oxide, were dispersed in 500 parts by weight of deionized water, and ultrasonicated for 30 minutes. Then, 2 parts by weight of a dispersant, sodium dodecylbenzene sulfonate, were added, and the mixture was placed in a water bath at 80° C., magnetically stirred for 60 minutes, filtered, and dried at 110° C. for 6 hours to obtain A4;

[0050] (2) dissolving 400 parts by weight of Ho(NO3)3·6H2O in 500 parts by weight of deionized water, and then adding an appropriate amount of pH adjuster-nitric acid until the pH value of the final Ho(NO3)3 solution is 2, to obtain B4;

[0051] (3) A4 was dispersed in 60 parts by weight of a complexing agent, ethylenediamine, placed in an oil bath at 120° C., and magnetically stirred for 60 min to obtain C4;

[0052] (4) C4 was added dropwise to B4 at a rate of 1 mL / min, stirred and refluxed in an oil bath at 120°C for 120 min, and then the precipitate was collected by filtration using a Buchner funnel, rinsed three times with deionized water, and then dried in an oven at 110°C for 6 h to obtain D4;

[0053] (5) D4 was placed in a muffle furnace and calcined at 1100° C. for 2 h to obtain the green leaf-like spectrum rare earth pigment composition E4.

[0054] Example 5

[0055] (1) 100 parts by weight of Cr2O3 and 8 parts by weight of a spectrum modifier, nickel oxide, were dispersed in 500 parts by weight of deionized water, ultrasonicated for 30 minutes, and then 4 parts by weight of a dispersant, polyethylene glycol (PEG), were added, placed in a 70° C. water bath, magnetically stirred for 60 minutes, filtered, and dried at 100° C. for 12 hours to obtain A5;

[0056] (2) dissolving 400 parts by weight of PrCl3·6H2O in 500 parts by weight of deionized water, and then adding an appropriate amount of pH adjuster-nitric acid until the pH value of the final PrCl3 solution is 1, to obtain B5;

[0057] (3) A5 was dispersed in 50 parts by weight of complexing agent-urea, placed in an oil bath at 100° C., and magnetically stirred for 30 min to obtain C5;

[0058] (4) C5 was added dropwise to B5 at a rate of 0.5 mL / min, and the mixture was stirred and refluxed in an oil bath at 100°C for 90 min. The precipitate was collected by filtration using a Buchner funnel, and rinsed three times with deionized water, and then dried in an oven at 100°C for 6 h to obtain D5.

[0059] (5) D5 was placed in a muffle furnace and calcined at 900° C. for 2 h to obtain a green leaf spectrum rare earth pigment composition E5 (eg Figures 1 to 3 shown).

[0060] Comparative Example 1

[0061] Pure chromium oxide (Cr2O3), F1

[0062] Comparative Example 2

[0063] Pure europium chloride G1, dysprosium chloride G2, erbium nitrate G3, holmium nitrate G4, praseodymium chloride G5

[0064] Comparative Example 3

[0065] (1) 100 parts by weight of Cr2O3 and 8 parts by weight of a spectrum modifier, nickel oxide, were dispersed in 500 parts by weight of deionized water, ultrasonicated for 30 minutes, and then 4 parts by weight of a dispersant, polyethylene glycol (PEG), were added, placed in a 70° C. water bath, magnetically stirred for 60 minutes, filtered, and dried at 100° C. for 12 hours to obtain A5;

[0066] (2) A5 was dispersed in 50 parts by weight of complexing agent-urea, placed in an oil bath at 100° C., magnetically stirred for 30 min, and then filtered and dried to obtain C5;

[0067] (3) C5 was placed in a muffle furnace and calcined at 900° C. for 2 h to obtain a comparative pigment composition H1.

[0068] The following is a comparison of the effects of the green leaf spectrum rare earth pigment composition of the above embodiment and the comparative example:

[0069]

[0070]

[0071] Evaluation of the green leaf spectral effect: The more + signs there are, the better the bionic effect.

[0072] The above description is only a preferred embodiment of the present invention, and therefore cannot be used to limit the scope of the present invention. That is, equivalent changes and modifications made according to the patent scope of the present invention and the contents of the specification should still fall within the scope of the present invention.

Claims

1. A rare earth pigment composition imitating green leaf spectrum, characterized in that: It is prepared by mixing chromium oxide, rare earth compound, spectrum regulator, dispersant, complexing agent, pH regulator and deionized water, wherein: The rare earth compound is selected from rare earth oxide, rare earth chloride and rare earth nitrate, wherein the rare earth element is selected from gadolinium, praseodymium, europium, dysprosium, holmium and erbium.

2. A green leaf-like spectrum rare earth pigment composition as claimed in claim 1, characterized in that: The rare earth element is selected from praseodymium, dysprosium, holmium and erbium.

3. A green leaf-like spectrum rare earth pigment composition as claimed in claim 2, characterized in that: The rare earth compound is selected from ErCl3·6H2O, DyCl3·6H2O, Er(NO3)3·6H2O, Ho(NO3)3·6H2O and PrCl3·6H2O.

4. The green leaf-like spectrum rare earth pigment composition according to claim 1, characterized in that: The spectrum modifier is selected from zinc oxide, cobalt oxide and nickel oxide.

5. The green leaf-like spectrum rare earth pigment composition according to claim 1, characterized in that: The dispersant is selected from polyvinyl pyrrolidone, polyvinyl alcohol, sodium dodecylbenzene sulfonate and polyethylene glycol.

6. A green leaf-like spectrum rare earth pigment composition as claimed in claim 1, characterized in that: The complexing agent is selected from citric acid, ethylenediaminetetraacetic acid, pyrophosphoric acid, ethylenediamine and urea.

7. The green leaf spectrum rare earth pigment composition according to claim 1, characterized in that: The pH adjuster is selected from hydrochloric acid and nitric acid.

8. The green leaf spectrum rare earth pigment composition according to claim 1, characterized in that: The rare earth compound is PrCl3·6H2O, the spectrum regulator is nickel oxide, the dispersant is polyethylene glycol, the complexing agent is urea, and the pH regulator is nitric acid.

9. A green leaf spectrum rare earth pigment composition as claimed in any one of claims 1 to 8, characterized in that: The mass ratio of the chromium oxide, the rare earth compound, the spectrum regulator, the dispersant and the complexing agent is 100:60-100:5-10:1-5:30-100.

10. A method for preparing a green leaf spectrum rare earth pigment composition according to any one of claims 1 to 9, characterized in that: The steps include: (1) Dispersing Cr2O3 powder and spectrum modifier in deionized water, ultrasonicating for 10-60 min, then adding dispersant, stirring at 60-90°C for 30-90 min, filtering, and drying at 80-120°C for 4-12 h to obtain material A; (2) dissolving the rare earth compound in deionized water, and then adding a pH adjuster to a pH of 1-3 to obtain material B; (3) dispersing material A in a complexing agent, stirring at 100-150° C. for 30-90 min, to obtain material C; (4) Material C is added dropwise to material B, stirred and refluxed at 100-150°C for 30-120 min, and then the precipitate is collected, washed with deionized water, and dried at 80-120°C for 4-12 h to obtain material D; (5) Calcine material D at 600-1100°C for 1-3h to obtain.

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