CN105110375B - Infrared and chromic oxide-based pigment of visual camouflage and preparation method thereof - Google Patents
Infrared and chromic oxide-based pigment of visual camouflage and preparation method thereof Download PDFInfo
- Publication number
- CN105110375B CN105110375B CN201510420635.1A CN201510420635A CN105110375B CN 105110375 B CN105110375 B CN 105110375B CN 201510420635 A CN201510420635 A CN 201510420635A CN 105110375 B CN105110375 B CN 105110375B
- Authority
- CN
- China
- Prior art keywords
- pigment
- oxide
- based pigment
- infrared
- chromic oxide
- 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.)
- Active
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a kind of infrared and chromic oxide-based pigment of visual camouflage and preparation method thereof, chemical formula is CoyTizCr2xO3x+y+2z, y+z=0.05x~0.1x, wherein y=(0~0.5) z.Chromic oxide-based pigment is green, with loose structure.The present invention uses molten salt process, and carrier, titanium, cobalt improved chromium oxide are made using sodium chloride, by adjusting titanium pigment form and aspect are adjusted with the content of cobalt, using the recombination reaction of metal oxide, synthesis has the chromic oxide-based pigment approximate with chlorophyll color, and pigment is loose structure.Therefore while the pigment obtained by the present invention has pigment coloring function, due to the loose structure in granules of pigments so that pigment has good heat shielding；The specific infrared emissivity of the coating configured using pigment of the invention is decreased obviously.
Description
Technical field
The present invention relates to a kind of pigment, specific design a kind of infrared and the chromic oxide-based pigment of visual camouflage and its preparation side
Method.
Background technology
Chrome oxide green is a kind of important inorganic pigment, have the advantages that it is corrosion-resistant, fast light, wear-resisting because it has closely
Like the color and luster of plant chlorophyll, it is widely used in camouflage coating material.With continuing to develop for imaging technique, although this kind of
Camouflage paint has the green of allochlorophyll in visible region, and new infrared detecting set still can be according to them infrared
Greatest differences of the area with chlorophyll on reflectivity are screened.Therefore need to develop a kind of pigment, keeping chromium oxide pigments
Can infrared camouflage while green hue.
Current technology means are mainly with chromium oxide as primary raw material, and the different oxides that adulterate are changed after being calcined
The corundum structure solid solution of property.
Such as Chinese patent literature CN104445409A (application number 201310415524.2) discloses one kind by hydration oxygen
Change the method that chromium prepares the chromic oxide-based pigment of near-infrared high reflection.The invention is and a certain proportion of with hydrated chromium oxide as raw material
After additive is well mixed, in being calcined under high temperature, chromic oxide-based pigment is obtained；The additive be vanadic anhydride, aluminum oxide,
One kind or at least two mixture in aluminium hydroxide, titanium dioxide or iron oxide.The near-infrared of gained chrome oxide green pigment
More than 85%, products obtained therefrom has near infrared reflectivity high to reflectivity while chromium oxide pigments green hue is kept.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of infrared and the chromic oxide-based pigment of visual camouflage and its system
Preparation Method.
The technical scheme for realizing the object of the invention is a kind of infrared and chromic oxide-based pigment of visual camouflage, and its feature exists
In：Chemical formula is CoyTizCr2xO3x+y+2z, y+z=0.05x~0.1x, wherein y=(0~0.5) z.
Above-mentioned chromic oxide-based pigment has loose structure.
A kind of infrared preparation method with the chromic oxide-based pigment of visual camouflage as described above, reaction equation is as follows：
Comprise the following steps：
1) cobalt oxide, titanium dioxide, chromium oxide and the NaCl that will be weighed according to stoichiometric proportion are added in reactor, make thing
Reactor is sealed after material is well mixed.
2) heating makes step 1) temperature of charge that mixes rises to 900 DEG C~1000 DEG C, melted at 900 DEG C~1000 DEG C anti-
Answer 5~6 hours；After reaction terminates, the composite oxides obtained after being reacted with the soft water chilling without any mechanical admixture；It is rapidly cold
But the composite oxides after are first washed to ion concentration with the clean soft water of mechanical impurity and dropped in terms of NaCl after 0.5g/L,
Be washed with deionized again, until in nano composite oxide the content of final water-soluble salt in terms of NaCl in below 0.05g/L.
3) by step 2) cleaned the composite oxides after water-soluble salt crush after vacuum drying obtain it is infrared with it is visible
Light pretends chromic oxide-based pigment.
Y+z=0.05x~0.1x in above-mentioned reaction equation, wherein y=(0~0.5) z.
Above-mentioned steps 2) chilling rate of temperature fall be 100 DEG C/min~200 DEG C/min.
Above-mentioned steps 3) after vacuum drying, crushing obtains moisture in chromic oxide-based pigment and is less than 0.05wt%.
The present invention has positive effect：(1) present invention uses molten salt process, and carrier, titanium, cobalt improved oxygen are made using sodium chloride
Change chromium, pigment form and aspect are adjusted with the content of cobalt by adjusting titanium, using the recombination reaction of metal oxide, synthesis has green with leaf
The approximate chromic oxide-based pigment of plain color；The sodium chloride that reaction terminates to wrap up in rear product is dissolved in the water removal, the face for obtaining
Expect to be loose structure.Therefore the pigment obtained by the present invention is while have pigment coloring function, due to granules of pigments in it is many
Pore structure so that pigment has good heat shielding；The specific infrared emissivity of the coating configured using pigment of the invention is bright
It is aobvious to decline.
(2) in pigment preparation process of the invention, cobalt produces vacant structure and distortion of lattice with titanium so that obtained chromium base
Pigment not only chromatogram closer to chlorophyll, and due to lattice defect produce electron transfer so that infra-red radiation ability enters one
Step lifting, infrared reflectivity is approximate with leaf green.
(3) its is infrared than radiation, cooling work(of environment after the coating film forming being formulated using chromium base pigment of the invention
Can be significantly improved compared with existing infrared camouflage coating material.
Specific embodiment
The raw materials used purity of following examples is more than 99.5%.
(embodiment 1)
The chromic oxide-based pigment of infrared and visual camouflage of the present embodiment is composite oxides, and chemical formula is
CoyTizCr2xO3x+y+2z, prepare reaction equation as follows：
The mass fraction proportioning of each reactant is as follows during preparation：
Cobalt oxide 0.75；Titanium dioxide 8；Chromium oxide 167.2；NaCl 351.9.
The preparation method of the chromic oxide-based pigment of infrared and visual camouflage of the present embodiment is comprised the following steps：
1) in rotatable roller stainless steel reactor, add the cobalt oxide of above-mentioned metering, titanium dioxide, chromium oxide and
Pure NaCl is analyzed, and rotating cylinder makes reactor to be sealed after material is well mixed in reactor.
2) heating makes step 1) temperature of charge that mixes rises to 900 DEG C~930 DEG C, frit reaction 6 hours at such a temperature.
After reaction terminates, the composite oxides obtained after being reacted with the soft water chilling without any mechanical admixture, the speed of the cooling of chilling
It is 150 DEG C/min (150 DEG C of decline per minute) that the temperature of material is 55 DEG C~80 DEG C after chilling；It is first miscellaneous with mechanical after chilling
The clean soft water washing of matter, temperature is 55 DEG C~58 DEG C during washing, after dropping to 0.5g/L (in terms of NaCl) to ion concentration, then
Be washed with deionized, until in composite oxides the content of final water-soluble salt in 0.05g/L (in terms of NaCl) below.During washing
It refers to that soft water is 55 DEG C~58 DEG C with the temperature of material after soft water wants the material after chilling to contact that temperature is 55 DEG C.
3) by step 2) cleaned the composite oxides after water-soluble salt carry out vacuum drying, crushing obtain infrared and visible ray
Pretend chromic oxide-based pigment.90 DEG C~100 DEG C of drying temperature, powder pigment moisture is controlled in 0.05% (mass parts) below.
(embodiment 2)
The mass fraction proportioning of each reactant is as follows when prepared by the present embodiment：
Cobalt oxide 1.5；Titanium dioxide 8；Chromium oxide 182.4；NaCl 383.8.
Remaining is same as Example 1 for the preparation method of the chromic oxide-based pigment of infrared and visual camouflage of the present embodiment, no
It is with part：
Step 2) in material frit reaction 5.5 hours at 940 DEG C in reactor.
After reaction terminates, with the soft water chilling without any mechanical admixture, the rate of temperature fall of chilling is 180 DEG C/min, cooling
First washed with the clean soft water of mechanical impurity afterwards, wash temperature is 54 DEG C.
Step 3) 90 DEG C of drying temperature.
(embodiment 3)
The mass fraction proportioning of each reactant is as follows when prepared by the present embodiment：
Cobalt oxide 2.25；Titanium dioxide 8.0；Chromium oxide 197.6；NaCl 207.9.
Remaining is same as Example 1 for the preparation method of the chromic oxide-based pigment of infrared and visual camouflage of the present embodiment, no
It is with part：
Step 2) in reactor material in 980 DEG C of frit reactions 5.2 hours.
Chilling but after first washed with the clean soft water of mechanical impurity after filtering, wash temperature be 50 DEG C.
Step 3) in 98 DEG C of drying temperature.
(embodiment 4)
The mass fraction proportioning of each reactant is as follows when prepared by the present embodiment：
Cobalt oxide 3；Titanium dioxide 8；Chromium oxide 212.8；NaCl 223.8
Remaining is same as Example 1 for the preparation method of the chromic oxide-based pigment of infrared and visual camouflage of the present embodiment, no
It is with part：
Step 2) in reactor material in 1000 DEG C of frit reactions 5 hours.
After reaction terminates, with the soft water chilling without any mechanical admixture, chilling rate of temperature fall is 120 DEG C/min, after cooling
First washed with the clean soft water of mechanical impurity after filtering, wash temperature is 57 DEG C.
Step 3) 93 DEG C of drying temperature.
(embodiment 5)
The mass fraction proportioning of each reactant is as follows when prepared by the present embodiment：
Cobalt oxide 3.75；Titanium dioxide 8；Chromium oxide 228；NaCl 239.8.
Remaining is same as Example 1 for the preparation method of the chromic oxide-based pigment of infrared and visual camouflage of the present embodiment, no
It is with part：
Step 2) in reactor material in 920 DEG C of frit reactions 5.6 hours.
After reaction terminates, with the soft water chilling without any mechanical admixture, chilling rate of temperature fall is 130 DEG C/min.
First washed with the clean soft water of mechanical impurity after filtering after cooling, wash temperature is 59 DEG C.
Step 3) 100 DEG C of drying temperature.Chromic oxide-based pigment obtained by embodiment 1 to embodiment 5 is detected, is tied
Fruit is as follows：
Wherein infrared emittance is the emissivity in 8 to 12 microns of infrared band wavelength, and detecting instrument is using peace continent science and technology
ET-10 portable infrared spectral emissions instrument measurement, 8-12 μm of wave-length coverage.
The present invention uses molten salt process, and carrier is made using sodium chloride, titanium, cobalt improved chromium oxide, by adjusting containing for titanium and cobalt
Amount adjustment pigment form and aspect, using the recombination reaction of metal oxide, synthesis has the chromic oxide-based face approximate with chlorophyll color
Material；The sodium chloride that reaction terminates to wrap up in rear product is dissolved in the water removal, and the pigment for obtaining is loose structure.Therefore it is of the invention
While obtained pigment has pigment coloring function, due to the loose structure in granules of pigments so that pigment has good
Heat shielding；The specific infrared emissivity of the coating configured using pigment of the invention is decreased obviously.
In other pigment preparation process of the invention, cobalt produces vacant structure and distortion of lattice with titanium so that obtained chromium
Base pigment not only chromatogram closer to chlorophyll, and due to lattice defect produce electron transfer so that infra-red radiation ability is entered
One step is lifted, and infrared reflectivity is approximate with leaf green.
Claims (3)
1. a kind of infrared preparation method with the chromic oxide-based pigment of visual camouflage, it is characterised in that：Prepared is chromic oxide-based
Pigment has loose structure, and chemical formula is CoyTizCr2xO3x+y+2z, y+z=0.05x~0.1x, wherein y=（0~0.5）z；
Reaction equation is as follows：
Preparation method is comprised the following steps：
1）0.75 part of the cobalt oxide that will be weighed according to mass fraction, 8 parts of titanium dioxide, 167.2 parts and NaCl 351.9 of chromium oxide
Part is added in reactor, makes to seal reactor after material is well mixed；
2）Heating makes step 1）The temperature of charge of mixing rises to 900 DEG C~1000 DEG C, the frit reaction 5 at 900 DEG C~1000 DEG C
~6 hours；After reaction terminates, the composite oxides obtained after being reacted with the soft water chilling without any mechanical admixture；Rapidly cool down
Composite oxides afterwards are first washed to ion concentration with the clean soft water of mechanical impurity and dropped in terms of NaCl after 0.5g/L, then
Be washed with deionized, until in nano composite oxide the content of final water-soluble salt in terms of NaCl in below 0.05g/L；
3）By step 2）The composite oxides after water-soluble salt are cleaned and crush after vacuum drying and obtained infrared pseudo- with visible ray
Fill chromic oxide-based pigment.
2. the infrared preparation method with the chromic oxide-based pigment of visual camouflage according to claim 1, it is characterised in that：Step
Rapid 2）The rate of temperature fall of chilling is 100 DEG C/min~200 DEG C/min.
3. the infrared preparation method with the chromic oxide-based pigment of visual camouflage according to claim 1, it is characterised in that：Step
Rapid 3）After vacuum drying, moisture is less than 0.05wt% during crushing obtains chromic oxide-based pigment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510420635.1A CN105110375B (en) | 2015-07-20 | 2015-07-20 | Infrared and chromic oxide-based pigment of visual camouflage and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510420635.1A CN105110375B (en) | 2015-07-20 | 2015-07-20 | Infrared and chromic oxide-based pigment of visual camouflage and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105110375A CN105110375A (en) | 2015-12-02 |
| CN105110375B true CN105110375B (en) | 2017-06-23 |
Family
ID=54658547
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510420635.1A Active CN105110375B (en) | 2015-07-20 | 2015-07-20 | Infrared and chromic oxide-based pigment of visual camouflage and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105110375B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107758744A (en) * | 2017-11-16 | 2018-03-06 | 华南协同创新研究院 | A kind of camouflage chromium oxide viridine green and preparation method thereof |
| CN116120763A (en) * | 2022-12-31 | 2023-05-16 | 石家庄市油漆厂 | Green hyperspectral camouflage inorganic pigment and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102826839B (en) * | 2012-09-17 | 2013-10-30 | 电子科技大学 | Green near infrared reflection pigment and preparation method of green near infrared reflection pigment |
| CN103922394B (en) * | 2014-04-12 | 2016-03-02 | 中国科学院新疆理化技术研究所 | The preparation method of a kind of overlong nanowire structure and nano belt structure CaCu 3 Ti 4 O |
-
2015
- 2015-07-20 CN CN201510420635.1A patent/CN105110375B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN105110375A (en) | 2015-12-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Raj et al. | Terbium doped Sr2MO4 [M= Sn and Zr] yellow pigments with high infrared reflectance for energy saving applications | |
| Masui et al. | Novel and environmentally friendly (Bi, Ca, Zn) VO4 yellow pigments | |
| Thongkanluang et al. | Preparation and characterization of Cr2O3–TiO2–Al2O3–V2O5 green pigment | |
| Liu et al. | The evaluation of thermal performance of cool coatings colored with high near-infrared reflective nano-brown inorganic pigments: Magnesium doped ZnFe2O4 compounds | |
| Sreeram et al. | Cerium molybdenum oxides for environmentally benign pigments | |
| Sadeghi-Niaraki et al. | Preparation of (Fe, Cr) 2O3@ TiO2 cool pigments for energy saving applications | |
| Thejus et al. | Rational approach to synthesis low-cost BiVO4–ZnO complex inorganic pigment for energy efficient buildings | |
| Ozel et al. | Production of coloured zircon pigments from zircon | |
| Melo et al. | Lanthanum cobaltite black pigments with perovskite structure | |
| Liang et al. | Preparation of Cr2O3-based pigments with high NIR reflectance via thermal decomposition of CrOOH | |
| Geng et al. | Optimization design of CuCrxMn2− xO4-based paint coatings used for solar selective applications | |
| Zhou et al. | Synthesis of high near infrared reflection wurtzite structure green pigments using Co-doped ZnO by combustion method | |
| CN105110375B (en) | Infrared and chromic oxide-based pigment of visual camouflage and preparation method thereof | |
| Chen et al. | Environmental-friendly yellow pigments based on Zr doped Y4MoO9 | |
| JP5554541B2 (en) | Infrared reflective material, method for producing the same, and paint and resin composition containing the same | |
| Du et al. | Synthesis and characterization of black ceramic pigments by recycling of two hazardous wastes | |
| Marques et al. | Synthesis of yttrium aluminate doped with Cr3+ using MgF2–Na2B4O7 as mineralizers to obtain red pigments for ceramic tiles application | |
| He et al. | Synthesis and coloration of highly dispersive SiO2/BiVO4 hybrid pigments with low cost and high NIR reflectance | |
| CN110878179B (en) | Black heat-reflective pigment and preparation method and application thereof | |
| Chen et al. | Cr and Mg co-doped YAlO3 red cool pigments with high NIR reflectance and infrared emissivity for sustainable energy-saving applications | |
| Wang et al. | Thermal insulation performance of novel orange fabric coated with Fe3+-doped La2Zr2O7 NIR solar reflectivity pigment | |
| US20170198145A1 (en) | Inorganic blue pigments from cobalt doped magnesium having transition element oxides and a process for the preparing the same | |
| Zhang et al. | Amino-acid-assisted preparation of CoAl2O4/kaolin hybrid pigments | |
| Abraham et al. | Bi1. 7V8O16: the first Bi-Hollandite-type compound | |
| Partl et al. | High temperature stable bismuth vanadate composite pigments via vanadyl-exchanged zeolite precursors |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |