CN115196678A - Chromium (III) -doped high near-infrared reflection inorganic pigment and preparation method and application thereof - Google Patents

Chromium (III) -doped high near-infrared reflection inorganic pigment and preparation method and application thereof Download PDF

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CN115196678A
CN115196678A CN202110390957.1A CN202110390957A CN115196678A CN 115196678 A CN115196678 A CN 115196678A CN 202110390957 A CN202110390957 A CN 202110390957A CN 115196678 A CN115196678 A CN 115196678A
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pigment
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phase sintering
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孙晓琦
肖瑜
黄彬
冯罗
谢文琦
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Xiamen Institute of Rare Earth Materials
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    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G37/00—Compounds of chromium
    • C01G37/006—Compounds containing, besides chromium, two or more other elements, with the exception of oxygen or hydrogen
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09C1/346—Chromium oxides
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/64—Optical properties, e.g. expressed in CIELAB-values b* (yellow-blue axis)
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    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/66—Hue (H*)

Abstract

The invention discloses a chromium (III) -doped high near-infrared reflection inorganic pigment and a preparation method and application thereof, wherein the chemical general formula of the pigment is Bi 3 Y 1‑x Cr x O 6 (x is more than 0 and less than or equal to 0.5), the color of the pigment can be changed from light yellow to brick red by changing the doping amount of Cr (III), and the pigment still has high near infrared reflectivity (higher than 90 percent) when the color of the pigment is deepened to deep brick red so as to effectively reflect the solar radiation energy. The pigment prepared by the invention can be widely used in the fields of cosmetics, building exterior walls, ship decks, aerospace, oil tank storage tanks and the like (such as chemical product storage tank coatings, vehicle and ship heat insulation coatings, metal sheet heat insulation coatings, communication base station heat insulation coatings, building exterior wall coatings and the like) so as to meet the color requirements of people,and as a cooling material. Meanwhile, the process for preparing the pigment is simple, the equipment requirement is low, and industrial production can be realized.

Description

Chromium (III) -doped high near-infrared reflection inorganic pigment and preparation method and application thereof
Technical Field
The invention belongs to the field of inorganic oxide pigments, and particularly relates to a high near-infrared reflection inorganic pigment (Bi) 3 Y 1- x Cr x O 6 Inorganic pigments) and methods of making and using the same.
Background
At present, human resources are in short supply, and thus, a plurality of researchers are stimulated to develop and utilize solar energy. However, sunlight also generates energy radiation to buildings and the like, and excessive heat accumulated on the surfaces of the buildings even causes a heat island effect, thereby bringing inconvenience to human life. In order to balance the poor circulation caused by the heat island effect, extra energy is added for cooling, such as the use of a large number of central air conditioners and cooling equipment, so that a new heat tide of an energy saving concept is promoted. The pigment is a novel energy-saving environment-friendly material and can reflect most of near-infrared radiation, so that the pigment has higher solar reflectivity, and can achieve obvious heat insulation and cooling effects by being made into a coating and coated on the surface of an object. Therefore, the coating can be used for the inner and outer wall surfaces of a building in a hot-summer and cold-winter area to make the interior of the building warm in winter and cool in summer, so that the accumulation of building energy and the load of a cooling system are reduced, the use of cooling equipment such as an air conditioner is reduced, the urban 'heat island effect' is relieved, the energy is saved, and the sustainable development strategy of the energy is realized.
In recent years, the development of high near infrared reflective materials has attracted a great deal of attention from researchers. Meanwhile, under the guidance of the green environmental protection concept, the high solar reflective pigment is rapidly developing. Inorganic pigments show greater advantages in chemical resistance, hiding power and weather resistance than organic pigments.
Has high near infrared reflectivityEnergetic TiO 2 The white pigment is considered to be the best and most important white pigment in the world at present, but is limited by single color, so that the visual enjoyment and color performance requirements of people on color cannot be met. Various color pigments are also in use, and at present, yellow pigment is the most reported inorganic pigment, such as a series of bismuth vanadate-Based (BiVO) reported by Indian experts 4 -CaMoO 4 ，(LiLaZn) 1/3 MoO 4 -BiVO 4 ，Li 0.1 RE 0.1 Bi 0.8 Mo 0.2 V 0.8 O 4 ) The yellow pigment generally has better color performance and higher near infrared reflection performance. Chinese researchers have also developed series of color pigments, such as Han Aijun topic group developing large red mica/gamma-Ce 2-x Y x S 3 Orange-yellow Fe-doped LaAlO 3 Color pigments of high reflectance. However, studies on the inorganic pigment of the haematochrome-like type are rare. At present, the red inorganic pigment is mainly iron oxide red, cadmium red, cerium sulfide and the like. However, the near infrared reflectance of iron oxide red pigments is relatively low; the cadmium red pigment contains highly toxic elements, so the cadmium red pigment can cause harm to human health; while the cerium sulfide pigment has good color performance, the cerium sulfide pigment is frequently used in high-end cosmetics due to the complex preparation process and higher cost. Therefore, how to develop the haematochrome-like pigment with good color performance, low cost and simple preparation process becomes a technical problem to be solved urgently.
Disclosure of Invention
In order to improve the technical problem, the invention provides a near infrared reflection pigment, wherein the chemical general formula of the pigment is as follows: bi 3 Y 1-x Cr x O 6 Wherein:
cr (III) is a doping element, x represents the doping molar quantity of Cr (III), and x is more than 0 and less than or equal to 0.5.
For example, 0 < x.ltoreq.0.05 or 0.05 < x.ltoreq.0.5; illustratively, x is 0.01, 0.02, 0.03, 0.04, 0.05, 0.08, 0.1, 0.2, 0.3, 0.4, 0.5.
According to the invention, the color of the pigment can be changed from light yellow to brick red by changing the doping molar amount of Cr (III).
According to the embodiment of the invention, when x is more than 0 and less than or equal to 0.05, the color of the near-infrared reflection pigment is yellow; when x is more than 0.05 and less than or equal to 0.5, the color of the pigment is brick red.
According to an embodiment of the invention, the near infrared reflective pigment has an average particle size of 2 to 10 μm, preferably 3 to 8 μm, exemplarily 2 μm, 3 μm, 5 μm, 8 μm, 10 μm.
According to an embodiment of the invention, the average near infrared reflectance of the near infrared reflective pigment is greater than 90%, such as 91 to 98%, illustratively 92%, 93%, 95%, 98%.
According to the embodiment of the invention, the near-infrared reflection pigment is prepared from raw materials comprising a Bi source, a Y source and a Cr source through a solid-phase sintering method.
According to an embodiment of the invention, the Bi source is provided by a Bi-containing compound. For example, provided by at least one of a carbonate, an oxide, a chloride, a nitrate, and a sulfate of a Bi-containing element; preferably from oxides containing Bi (e.g. Bi) 2 O 3 ) Provided is a method.
According to an embodiment of the invention, the Y source is provided by a compound containing the Y element; for example, provided by at least one of a carbonate, an oxide, a chloride, a nitrate, and a sulfate containing the Y element; preferably from oxides containing the element Y (e.g. Y) 2 O 3 ) Provided is a method.
According to an embodiment of the invention, the source of Cr is provided by a compound containing an element Cr; for example, provided by at least one of a carbonate, an oxide, a chloride, a nitrate, and a sulfate of a Cr-containing element; preferably from Cr-containing oxides (e.g. Cr) 2 O 3 ) Provided is a method.
According to an embodiment of the present invention, the near infrared reflective pigment may be Bi 3 Y 0.95 Cr 0.05 O 6 、Bi 3 Y 0.7 Cr 0.3 O 6 、Bi 3 Y 0.5 Cr 0.5 O 6 . Preferably, bi 3 Y 0.7 Cr 0.3 O 6 、Bi 3 Y 0.5 Cr 0.5 O 6 All the colors of the red bricks are brick red. Preferably, bi 3 Y 0.95 Cr 0.05 O 6 The color of (a) is orange yellow.
The invention also provides a preparation method of the near-infrared reflection pigment, which comprises the following steps:
bi source, Y source and Cr source are used as raw materials, and Bi is expressed by a chemical formula 3 Y 1-x Cr x O 6 And (x is more than 0 and less than or equal to 0.5), and the near-infrared reflection pigment is obtained by solid-phase sintering.
According to an embodiment of the present invention, the Bi, Y and Cr sources have the meaning as described above.
According to an embodiment of the invention, the temperature of the solid phase sintering is 700 ℃ to 1000 ℃, exemplary 700 ℃, 800 ℃, 900 ℃, 1000 ℃, preferably 900 ℃.
According to an embodiment of the invention, the time of the solid phase sintering is 240-600 min, exemplary 240min, 360min, 480min, 600min, preferably 480min.
According to an embodiment of the present invention, the temperature rise rate of the solid phase sintering is 1-10 ℃/min, illustratively 1 ℃/min, 5 ℃/min, 10 ℃/min, preferably 10 ℃/min.
According to an embodiment of the present invention, before the solid phase sintering process, the method further comprises a step of grinding the raw material. For example, the milling may be wet milling or ball milling; preferably, the medium used for milling may be at least one of acetone, water and ethanol, preferably acetone. Preferably, the time of the grinding is 2 to 6 hours, such as 2 hours, 4 hours, 6 hours. Further, the rotation speed of the grinding is 200-600 rpn/min.
According to an embodiment of the present invention, the preparation method further comprises a step of drying the ground raw material. For example, the drying temperature is 40 to 60 ℃, illustratively 40 ℃,50 ℃, 60 ℃, preferably 50 ℃. Further, the drying time may be 0.5 to 2 hours, illustratively 0.5 hour, 1.5 hour, 2 hours, and preferably 1 hour.
According to an embodiment of the present invention, the preparation method further comprises grinding the prepared calcined sample after the solid-phase sintering is completed. Preferably, the average particle size of the calcined sample after grinding is from 2 to 10 μm, preferably from 3 to 8 μm, exemplarily 2 μm, 3 μm, 5 μm, 8 μm, 10 μm.
According to an exemplary embodiment of the present invention, the preparation method comprises the steps of: according to the formula Bi 3 Y 1- x Cr x O 6 (x is more than 0 and less than or equal to 0.5), sequentially weighing a Bi source, a Y source and a Cr source, adding a grinding medium (such as acetone) for grinding, drying the ground mixture, carrying out solid-phase sintering treatment, and grinding the obtained calcined sample again to obtain the near-infrared reflection pigment with uniform particle size.
The invention also provides application of the near-infrared reflection pigment in the fields of cosmetics, building materials, coatings, plastics, vehicles, ship decks, aerospace, oil tank storage tanks or printing ink and the like.
Preferably, the near-infrared reflection pigment can be used for high-reflectivity coatings, such as coatings for preparing chemical storage tanks, thermal insulation coatings for vehicles and ships, thermal insulation coatings for metal plates, thermal insulation coatings for communication base stations or coatings for building exterior walls.
The invention has the advantages of
The invention prepares Bi with high near-infrared reflection 3 Y 1-x Cr x O 6 The inorganic pigment can change the color of the pigment from light yellow to brick red by changing the doping molar weight of Cr (III). And when the color of the pigment is darkened, the near infrared reflectivity of the pigment can still reach more than 90 percent. The pigment prepared by the invention can be widely used in the fields of cosmetics, building exterior walls, ship decks, aerospace, oil tank storage tanks and the like, can meet the color requirements of people, and can be used as a cool material. Meanwhile, the process for preparing the pigment is simple, the equipment requirement is low, and industrial production can be realized.
Drawings
FIG. 1 shows Bi prepared in example 1 3 Y 0.7 Cr 0.3 O 6 And Bi obtained in example 2 3 Y 0.5 Cr 0.5 O 6 XRD pattern of pigment.
FIG. 2 shows Bi prepared in example 1 3 Y 0.7 Cr 0.3 O 6 And Bi obtained in example 2 3 Y 0.5 Cr 0.5 O 6 A near infrared reflectance spectrum of the pigment.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to specific embodiments. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
In the following examples of the present invention, the purity of both bismuth oxide and chromium oxide was 99%, both of which were purchased from Aladdin reagents, inc. Yttria (99.99%) was purchased from Jiangxiang province as a new material technology corporation.
The structural characteristics of the synthesized sample are analyzed by adopting a Japanese physical X-ray diffractometer, and the scanning range is as follows: 10-80 °, scanning speed: 10 °/min, step size: 0.02 °/s, 40kV and 15mA operating voltage and current, respectively.
The near-infrared reflection performance of the pigment is measured by adopting an ultraviolet-visible-near-infrared spectrophotometer of Agilent 5000 in America, a reference white plate is made of Polytetrafluoroethylene (PTFE), a powder sample is put into a transparent container for testing, and the measurement is carried out within the range of 200nm-2500nm in the step length of 1 nm. The solar reflectance (R) was calculated according to the G173-03 standard set by the American Society for Testing and Materials (ASTM) by the formula:
Figure BDA0003016679410000051
wherein r (λ) and i (λ) represent the reflectance of the sample at the wavelength λ and the standard radiation intensity (W.m), respectively -2 ·nm -1 )。
The color coordinates of the pigment sample are recorded by a Hangzhou CS-580A spectrophotometer, the light source is CLEDs, and the color system is regulated according to CIE1976-L a b color system of the International Commission on illumination (CIE), L represents the brightness of the sample and the value ranges from 0 (black) to 100 (white), wherein a represents the red-green color property of the pigment and the value ranges from-128 to 128, negative a represents green, and positive represents red; b represents the pigment blue Huang Xingzhi, ranging from-128 to 128, negative b represents blue, positive b represents yellow, and parameter C represents the pigment color saturation in addition to Lab, C is calculated as = [ (a) 2 +(b*) 2 ] 1/2 。
Examples 1 to 2
Examples 1-2 pigments were synthesized by a solid phase sintering method, and the difference between the examples is the amount of raw materials, wherein table 1 lists the kinds and amounts of raw materials used in the examples.
The high near infrared reflection inorganic pigment has a chemical structural formula of Bi 3 Y 1-x Cr x O 6 (x =0.3 or 0.5), the specific preparation steps are as follows:
1) According to the formula Bi 3 Y 1-x Cr x O 6 (x =0.3 or 0.5) in the stoichiometric ratio of each element, and a Bi-containing compound, a Y-containing compound, and a Cr-containing compound are weighed respectively;
2) Adding the mixed powder weighed in the step 1) into a mortar, adding acetone, and grinding until most of the acetone is volatilized (the powder is not wet);
3) Transferring the powder in the step 2) into a crucible, then putting the crucible into an oven, and drying for 1h at 50 ℃;
4) Transferring the powder in the step 3) into a muffle furnace, heating to 900 ℃ at a heating rate of 10 ℃/min, then preserving heat for 6h, taking out the finally obtained calcined sample, and uniformly grinding to obtain a pigment sample, wherein the average particle size of the pigment sample is 3-8 μm.
Table 1 examples 1-2 preparation parameters
Examples Chemical formula of pigment Bi 2 O 3 (g) Y 2 O 3 (g) Cr 2 O 3 (g)
Example 1 Bi 3 Y 0.7 Cr 0.3 O 6 5 0.5653 0.1631
Example 2 Bi 3 Y 0.5 Cr 0.5 O 6 5 0.4038 0.2718
FIGS. 1 and 2 show Bi obtained in example 1-2 3 Y 1-x Cr x O 6 Structural properties and near infrared reflectance properties of the pigment samples. As can be seen in fig. 1, the pigment samples formed an intact solid solution upon calcination. As can be seen from fig. 2, the average near infrared reflectance of the pigment is higher than 90%. The color performance of the pigment tested by the color tester is Bi 3 Y 0.7 Cr 0.3 O 6 (L*＝48.21，a*＝34.31，b*＝31.75)；Bi 3 Y 0.5 Cr 0.5 O 6 (L × =49.13, a × =37.92, b × = 30.47), indicating that the pigment color is brick red.
Example 3
The preparation method is the same as example 1, except that: weighing Bi according to stoichiometric ratio 2 O 3 (5g)，Y 2 O 3 (0.7673g)，Cr 2 O 3 (0.0272 g) and Bi was prepared according to the method in example 1 3 Y 0.95 Cr 0.05 O 6 Pigment samples. The near infrared reflectance was measured to be 93%; color performance tests were performed on the pigment and the result was expressed as orange yellow (L × =60.50, a × =31.37, b × = 47.19), indicating that the pigment color was a yellow color system.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made without departing from the spirit and principle of the present invention shall fall within the protection scope of the present invention.

Claims (10)

1. A near-infrared reflective pigment, characterized in that said pigment has the general chemical formula: bi 3 Y 1-x Cr x O 6 Wherein:
cr (III) is a doping element, x represents the doping molar quantity of Cr (III), and x is more than 0 and less than or equal to 0.5.
For example, 0 < x.ltoreq.0.05 or 0.05 < x.ltoreq.0.5.
Preferably, when the near-infrared reflection pigment has x of more than 0 and less than or equal to 0.05, the color of the pigment is yellow; when x is more than 0.05 and less than or equal to 0.5, the color of the pigment is brick red.
2. The near-infrared reflective pigment of claim 1, wherein the near-infrared reflective pigment has an average particle diameter of 2 to 10 μm.
Preferably, the near infrared reflective pigment has an average near infrared reflectance of greater than 90%, such as from 91 to 98%.
3. The near-infrared reflective pigment according to claim 1 or 2, wherein the near-infrared reflective pigment is prepared from raw materials comprising a Bi source, a Y source, and a Cr source by a solid-phase sintering method.
4. The near-infrared reflective pigment of claim 3, wherein the source of Bi is provided by a compound comprising a Bi element. For example, by at least one of a carbonate, an oxide, a chloride, a nitrate and a sulfate of the Bi-containing element.
Preferably, the Y source is provided by a compound containing the Y element; for example, by at least one of a carbonate, an oxide, a chloride, a nitrate, and a sulfate containing the element Y.
Preferably, the source of Cr is provided by a compound containing a Cr element; for example, by at least one of a carbonate, an oxide, a chloride, a nitrate, and a sulfate of a Cr-containing element.
5. The near-infrared reflective pigment according to any one of claims 1 to 4, wherein the near-infrared reflective pigment is Bi 3 Y 0.95 Cr 0.05 O 6 、Bi 3 Y 0.7 Cr 0.3 O 6 、Bi 3 Y 0.5 Cr 0.5 O 6 。
6. The process for preparing a near-infrared reflective pigment according to any one of claims 1 to 5, characterized in that the process comprises the steps of:
bi source, Y source and Cr source are used as raw materials, and Bi is expressed by a chemical formula 3 Y 1-x Cr x O 6 And (x is more than 0 and less than or equal to 0.5), and the near-infrared reflection pigment is obtained by solid-phase sintering.
Preferably, the Bi, Y and Cr sources all have the meaning as defined in claim 4.
7. The method of claim 6, wherein the temperature of the solid phase sintering is 700 ℃ to 1000 ℃.
Preferably, the time for solid phase sintering is 240-600 min.
Preferably, the temperature rise rate of the solid-phase sintering is 1-10 ℃/min.
8. The method according to claim 6 or 7, further comprising a step of grinding the raw material before the solid-phase sintering treatment.
Preferably, the preparation method further comprises a step of drying the ground raw material. For example, the drying temperature is 40 to 60 ℃, and the drying time can be 0.5 to 2 hours.
Preferably, the preparation method further comprises the step of grinding the prepared calcined sample after the solid-phase sintering is completed. Preferably, the average particle size of the calcined sample after grinding is 2 to 10 μm.
9. The method of any one of claims 6 to 8, comprising the steps of: according to the formula Bi 3 Y 1-x Cr x O 6 (x is more than 0 and less than or equal to 0.5), sequentially weighing a Bi source, a Y source and a Cr source, adding a grinding medium for grinding, drying the ground mixture, performing solid-phase sintering treatment, and grinding the obtained calcined sample again to obtain the near-infrared reflection pigment with uniform particle size.
10. Use of the near-infrared reflective pigment according to any one of claims 1 to 5 and/or the near-infrared reflective pigment produced by the production process according to any one of claims 6 to 9 in the fields of cosmetics, building materials, coatings, plastics, vehicles, ship decks, aerospace, tank tanks or inks, and the like.
Preferably, the near-infrared reflection pigment can be used for high-reflectivity coatings, such as coatings for preparing chemical storage tanks, thermal insulation coatings for vehicles and ships, thermal insulation coatings for metal plates, thermal insulation coatings for communication base stations or coatings for building exterior walls.
CN202110390957.1A 2021-04-12 Chromium (III) -doped high near infrared reflection inorganic pigment and preparation method and application thereof Active CN115196678B (en)

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