CN115849886A - High near-infrared reflection blue inorganic pigment and preparation method thereof - Google Patents
High near-infrared reflection blue inorganic pigment and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of inorganic pigments, and particularly relates to a high near-infrared reflection blue inorganic pigment and a preparation method thereof. The general formula of the high near infrared reflection blue inorganic pigment is Zn 2‑ x Ni x SiO 4 Wherein x is more than 0 and less than or equal to 0.5. The preparation method comprises the following steps: first ZnO, siO 2 Mixing NiO serving as a raw material according to a stoichiometric ratio, grinding for 15-30min, tabletting under the pressure of 10-30MPa, maintaining the pressure for 1-5min, and finally heating to 1300-1500 ℃ in a box furnace at the heating rate of 5-10 ℃/min, wherein the sintering time is 2-6h, and the cooling rate is 5-10 ℃/min. Cooling to room temperature and grinding to obtain the blue inorganic pigment. The blue inorganic pigment synthesized by the invention is environment-friendly, nontoxic, bright in color, simple in preparation process, low in cost, short in preparation period and good in high-temperature performanceTemperature stability, chemical stability and high near infrared reflectance.
Description
Technical Field
The invention belongs to the technical field of inorganic pigments, and particularly relates to a high near-infrared reflection blue inorganic pigment and a preparation method thereof
Background
The pigment is a substance capable of dyeing objects, has the functions of decoration and protection, can be divided into organic pigment and inorganic pigment according to chemical compositions, and has bright color and strong tinting strength, but has poor stability and can not be used for a long time in a harsher environment, thereby limiting the application of the organic pigment. The inorganic pigment has excellent high-temperature stability, chemical stability, low price and better light resistance, heat resistance and solvent resistance than organic pigments, so that the inorganic pigment is widely applied to various fields of ceramics, plastics, fibers, glass, cement, rubber, coatings, glazes and the like and has important significance in production and life of people. Pigments can be divided into natural pigments and synthetic pigments according to their origin, the remainder being synthetic pigments, except for a few naturally occurring color-developing minerals.
At present, the blue inorganic pigment mainly comprises cobalt blue and ultramarine, and the cobalt blue contains cobalt element, is expensive and toxic, and cannot be widely applied in daily life; ultramarine (Na) 6 Al 4 Si 6 S 4 O 20 ) As the oldest blue pigment, although the pigment is environment-friendly and nontoxic, the pigment belongs to mineral pigments, has weak covering power and limited application range. Therefore, the blue inorganic pigment which does not contain heavy metal and has strong covering power is synthesized, the requirement of people on the environment-friendly nontoxic blue pigment can be met, and the application field of the blue inorganic pigment is widened.
Disclosure of Invention
The invention discloses a high near-infrared reflection blue inorganic pigment and a preparation method thereof, which are used for solving any one of the above and other potential problems in the prior art.
In order to achieve the purpose, the technical scheme of the invention is as follows: a blue inorganic pigment with high near infrared reflection has a chemical formula of Zn 2-x Ni x SiO 4 Wherein x is more than 0 and less than or equal to 0.5, zn is in a valence of +2, si is in a valence of +4, and Ni is in a valence of + 2.
Further, when x =0.05 the chemical formula of the blue inorganic pigment is Zn 1.95 Ni 0.05 SiO 4 The near infrared reflectance at 893nm was 90.7%, 85.8% at 1350 nm.
Further, when x =0.10 the chemical formula of the blue inorganic pigment is Zn 1.9 Ni 0.10 SiO 4 The near infrared reflectance at 893nm was 88.4% and 80.0% at 1350 nm.
Further, when x =0.15 the chemical formula of the blue inorganic pigment is Zn 1.85 Ni 0.15 SiO 4 The near infrared reflectance at 893nm was 84.6%, 72.1% at 1350 nm.
Further, when x =0.20 the chemical formula of the blue inorganic pigment is Zn 1.80 Ni 0.20 SiO 4 The near infrared reflectance at 893nm was 80.5%, 66.3% at 1350 nm.
Further, when x =0.30 the chemical formula of the blue inorganic pigment is Zn 1.70 Ni 0.30 SiO 4 The near infrared reflectance at 893nm was 80.0%, 75.8% at 1350 nm.
Another object of the present invention is to provide a method for preparing the above high near-infrared reflection blue inorganic pigment, specifically comprising the steps of:
s1) with ZnO, siO 2 NiO is used as a raw material, and the raw material is accurately weighed by an electronic balance according to the stoichiometric ratio of the pigment phase;
s2) putting the weighed powder raw materials in the S1) into an agate mortar, and manually grinding to fully mix the raw materials;
s3) putting the mixed raw materials obtained in the step S2) into a tabletting mold, and tabletting and forming by using a tabletting machine;
and S4) putting the block pressed and formed in the # S3) into a corundum crucible, and sintering at high temperature in a box-type furnace according to a temperature rise curve to obtain the blue high near-infrared reflection blue inorganic pigment with a single blue phase.
Further, the mass error of the raw material in the S1) is. + -. 0.0005g.
Further, the grinding time in the step S2) is 15-30min;
the diameter of the tabletting mold in the step S3) is 10-20mm, the pressure level of the pressing sample is 10-30MPa, and the pressure maintaining time is 1-5min.
Further, the temperature increase curve in S4) is:
firstly, heating to 1300-1500 ℃ according to the heating rate of 5-10 ℃/min, wherein the sintering time is 2-6h, and the sintering atmosphere is air;
then cooling according to the cooling rate of 5-10 ℃/min.
Further, the near infrared reflectivity of the high near infrared reflection blue inorganic pigment at 893nm is 80.5-90.7%, and the near infrared reflectivity at 1350nm is 66.3-85.8%.
Compared with the prior art, the invention has the following advantages:
(1) The blue inorganic pigment prepared by the invention has bright color, is environment-friendly and nontoxic, and the apparent color of the blue inorganic pigment can be regulated and controlled by the doping amount of Ni ions; the brightness L value of the blue inorganic pigment decreased from 70.7 to 56.32 with the increase of the content of the dopant ion, the a value increased from-2.62 to 0.16 and then decreased from 0.16 to-3.85 with the increase of the content of the dopant ion, the b value increased from-29.77 to-40.55 and then decreased from-40.55 to-33.25 with the increase of the content of the dopant ion, as shown in table 1.
(2) The blue inorganic pigment prepared by the invention has stable structure, good structural stability and chemical stability.
(3) The blue inorganic pigment prepared by the invention has high reflectivity in a near infrared region.
(4) The invention does not need to use a mineralizer, has simple process and can not introduce other ions due to the use of the mineralizer.
(5) The invention adopts manual grinding without using organic reagent, thereby reducing the harm to human body.
Drawings
Fig. 1 is a schematic diagram of XRD patterns of high near-infrared reflection blue inorganic pigments obtained in examples 1 to 5 using the preparation method of the present invention.
FIG. 2 is a schematic view of UV-Vis-NIR spectra of high near infrared reflection blue inorganic pigments obtained in examples 1 to 5 using the preparation method of the present invention.
Fig. 3 is a schematic view of the laa b spectra of the high nir blue inorganic pigments obtained in examples 1 to 5 according to the preparation method of the present invention.
Detailed Description
The present invention will be described in further detail below with reference to specific embodiments and the accompanying drawings. The examples are merely illustrative of the invention and do not limit the invention. It will be understood by those skilled in the art that various modifications and equivalents may be made to the embodiments of the present invention without departing from the spirit and scope of the invention, and such modifications and equivalents are within the scope of the invention.
The invention relates to a high near-infrared reflection blue inorganic pigment, wherein the chemical formula of the high near-infrared reflection blue inorganic pigment is Zn 2-x Ni x SiO 4 Wherein x is more than 0 and less than or equal to 0.5, zn is +2 valence, si is +4 valence, and Ni is +2 valence.
The method for preparing the high near-infrared reflection blue inorganic pigment specifically comprises the following steps:
s1) with ZnO, siO 2 NiO is used as a raw material, and the raw material is accurately weighed by an electronic balance according to the stoichiometric ratio of the pigment phase;
s2) putting the weighed powder raw materials in the S1) into an agate mortar, and manually grinding to fully mix the raw materials;
s3) putting the mixed raw materials obtained in the step S2) into a tabletting mold, and tabletting and forming by using a tabletting machine;
and S4) putting the block pressed and formed in the # S3) into a corundum crucible, and sintering at high temperature in a box type furnace according to a temperature rise curve to obtain the blue high near infrared reflection blue inorganic pigment with a single phase.
The mass error of the raw materials in the S1) is +/-0.0005 g.
The grinding time in the S2) is 15-30min;
the diameter of the tabletting mold in the S3) is 10-20mm, the pressure position of the pressing sample is 10-30MPa, and the pressure maintaining time is 1-5min.
The temperature rise curve in the step S4) is as follows:
firstly, heating to 1300-1500 ℃ according to the heating rate of 5-10 ℃/min, wherein the sintering time is 2-6h, and the sintering atmosphere is air;
then cooling according to the cooling rate of 5-10 ℃/min.
The near infrared reflectivity of the high near infrared reflection blue inorganic pigment at 893nm is 80.5-90.7%, and the reflectivity at 1350nm is 66.3-85.8%.
Example 1: preparation of 1g of Zn 1.95 Ni 0.05 SiO 4 Inorganic pigments
According to Zn 1.95 Ni 0.05 SiO 4 Respectively weighing ZnO (0.7132 g) and SiO by an electronic analytical balance according to a certain stoichiometric ratio 2 (0.2700 g), niO (0.0168 g), with a mass tolerance of. + -. 0.0005g. Pouring the weighed raw materials into an agate mortar, manually grinding for 20min, after grinding is finished, putting the mixed raw materials into a tabletting mold with the diameter of 15mm, pressurizing the mold through a tabletting machine, and maintaining the pressure for 3min under the pressure of 10 MPa. And (3) placing the pressed cylindrical block into a corundum crucible, then placing the corundum crucible into a box-type furnace, raising the temperature of the box-type furnace to 1400 ℃ at the heating rate of 5 ℃/min in the air atmosphere, preserving the heat for 2 hours at the temperature of 1400 ℃, after the heat preservation is finished, reducing the temperature to room temperature at the cooling rate of 5 ℃/min, and finally taking out a sample and grinding to obtain the stable blue inorganic pigment.
Example 2: preparation of 1g of Zn 1.9 Ni 0.1 SiO 4 Inorganic pigments
According to Zn 1.9 Ni 0.1 SiO 4 Respectively weighing ZnO (0.6596 g) and SiO by an electronic analytical balance according to a certain stoichiometric ratio 2 (0.2704 g), niO (0.0336 g), mass tolerance of. + -. 0.0005g. Pouring the weighed raw materials into an agate mortar, manually grinding for 20min, after grinding, putting the mixed raw materials into a tabletting mold with the diameter of 15mm, pressurizing the mold through a tabletting machine, and maintaining the pressure for 3min under the pressure of 10 MPa. And (3) placing the pressed cylindrical block into a corundum crucible, then placing the corundum crucible into a box furnace, raising the temperature of the box furnace to 1400 ℃ at the heating rate of 5 ℃/min in the air atmosphere, preserving the heat for 2 hours at the temperature of 1400 ℃, reducing the temperature to room temperature at the cooling rate of 5 ℃/min after the heat preservation is finished, and finally taking out a sample and grinding to obtain the stable blue inorganic pigment.
Example 3: preparation of 1g of Zn 1.85 Ni 0.15 SiO 4 Inorganic pigments
According to Zn 1.85 Ni 0.15 SiO 4 Respectively weighing ZnO (0.6787 g) and SiO by an electronic analytical balance according to a certain stoichiometric ratio 2 (0.2708 g), niO (0.0505 g), mass tolerance of. + -. 0.0005g. Pouring the weighed raw materials into an agate mortar, manually grinding for 20min, after grinding, putting the mixed raw materials into a tabletting mold with the diameter of 15mm, pressurizing the mold through a tabletting machine, and maintaining the pressure for 3min under the pressure of 10 MPa. And (3) placing the pressed cylindrical block into a corundum crucible, then placing the corundum crucible into a box furnace, raising the temperature of the box furnace to 1400 ℃ at the heating rate of 5 ℃/min in the air atmosphere, preserving the heat for 2 hours at the temperature of 1400 ℃, reducing the temperature to room temperature at the cooling rate of 5 ℃/min after the heat preservation is finished, and finally taking out a sample and grinding to obtain the stable blue inorganic pigment.
Example 4: preparation of 1g of Zn 1.8 Ni 0.2 SiO 4 Inorganic pigments
According to Zn 1.8 Ni 0.2 SiO 4 Respectively weighing ZnO (0.6613 g) and SiO by an electronic analytical balance according to a certain stoichiometric ratio 2 (0.2712 g), niO (0.0674 g), with a mass tolerance of. + -. 0.0005g. Pouring the weighed raw materials into an agate mortar, manually grinding for 20min, after grinding is finished, putting the mixed raw materials into a tabletting mold with the diameter of 15mm, pressurizing the mold through a tabletting machine, and maintaining the pressure for 3min under the pressure of 10 MPa. And (3) placing the pressed cylindrical block into a corundum crucible, then placing the corundum crucible into a box furnace, raising the temperature of the box furnace to 1400 ℃ at the heating rate of 5 ℃/min in the air atmosphere, preserving the heat for 2 hours at the temperature of 1400 ℃, reducing the temperature to room temperature at the cooling rate of 5 ℃/min after the heat preservation is finished, and finally taking out a sample and grinding to obtain the stable blue inorganic pigment.
Example 5: preparation of 1g of Zn 1.7 Ni 0.3 SiO 4 Inorganic pigments
According to Zn 1.7 Ni 0.3 SiO 4 Respectively weighing ZnO (0.6265 g) and SiO by an electronic analytical balance according to a certain stoichiometric ratio 2 (0.2721 g) and NiO (0.1015 g), with a mass tolerance of. + -. 0.0005g of the total weight. Pouring the weighed raw materials into an agate mortar, manually grinding for 20min, after grinding, putting the mixed raw materials into a tabletting mold with the diameter of 15mm, pressurizing the mold through a tabletting machine, and maintaining the pressure for 3min under the pressure of 10 MPa. And (3) placing the pressed cylindrical block into a corundum crucible, then placing the corundum crucible into a box furnace, raising the temperature of the box furnace to 1400 ℃ at the heating rate of 5 ℃/min in the air atmosphere, preserving the heat for 2 hours at the temperature of 1400 ℃, reducing the temperature to room temperature at the cooling rate of 5 ℃/min after the heat preservation is finished, and finally taking out a sample and grinding to obtain the stable blue inorganic pigment.
Table 1 is data of L a b:
the preparation method of the blue inorganic pigment with high near-infrared reflection provided by the embodiment of the application is described in detail above. The above description of the embodiments is only for the purpose of helping to understand the method of the present application and its core ideas; meanwhile, for a person skilled in the art, according to the idea of the present application, the specific implementation manner and the application scope may be changed, and in summary, the content of the present specification should not be construed as a limitation to the present application.
As used in the specification and claims, certain terms are used to refer to particular components. As one skilled in the art will appreciate, manufacturers may refer to a component by different names. This specification and claims do not intend to distinguish between components that differ in name but not function. In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. "substantially" means within an acceptable error range, that a person skilled in the art can solve the technical problem within a certain error range to substantially achieve the technical effect. The following description is of the preferred embodiment for carrying out the present application, but is made for the purpose of illustrating the general principles of the application and is not to be taken in a limiting sense. The protection scope of the present application shall be subject to the definitions of the appended claims.
It should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a good or system that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such good or system. Without further limitation, an element defined by the phrase "comprising a … …" does not exclude the presence of additional like elements in a commodity or system comprising the element.
It should be understood that the term "and/or" as used herein is merely one type of association that describes an associated object, meaning that three relationships may exist, e.g., a and/or B may mean: a exists alone, A and B exist simultaneously, and B exists alone. In addition, the character "/" herein generally indicates that the former and latter related objects are in an "or" relationship.
The foregoing description shows and describes several preferred embodiments of the present application, but as aforementioned, it is to be understood that the application is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the application as described herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the application, which is to be protected by the claims appended hereto.
Claims (10)
1. The high near-infrared reflection blue inorganic pigment is characterized in that the chemical formula of the high near-infrared reflection blue inorganic pigment is Zn 2-x Ni x SiO 4 Wherein x is more than 0 and less than or equal to 0.5, zn is in a valence of +2, si is in a valence of +4, and Ni is in a valence of + 2.
2. The blue inorganic pigment for high near-infrared reflection according to claim 1, wherein when x = iAt 0.05, the chemical formula of the blue inorganic pigment is Zn 1.95 Ni 0.05 SiO 4 The near infrared reflectance at 893nm was 90.7%, 85.8% at 1350 nm.
3. The blue high nir reflecting inorganic pigment according to claim 1, wherein the chemical formula of the blue inorganic pigment is Zn when x =0.10 1.9 Ni 0.10 SiO 4 The near infrared reflectance at 893nm was 88.4%, 80.0% at 1350 nm.
4. The high nir reflecting blue inorganic pigment according to claim 1, wherein the chemical formula of the blue inorganic pigment is Zn when x =0.15 1.85 Ni 0.15 SiO 4 The near infrared reflectance at 893nm was 84.6%, 72.1% at 1350 nm.
5. The blue high nir reflecting inorganic pigment according to claim 1, wherein the chemical formula of the blue inorganic pigment is Zn when x =0.20 1.80 Ni 0.20 SiO 4 The near infrared reflectance at 893nm was 80.5%, 66.3% at 1350 nm.
6. The high nir reflecting blue inorganic pigment according to claim 1, wherein the chemical formula of the blue inorganic pigment is Zn when x =0.30 1.70 Ni 0.30 SiO 4 The near infrared reflectance at 893nm was 80.0%, 75.8% at 1350 nm.
7. A process for preparing a blue inorganic pigment with high near-infrared reflectance according to any one of claims 1 to 6, characterized in that it comprises the following steps:
s1) with ZnO, siO 2 NiO is used as a raw material, and the raw material is accurately weighed by an electronic balance according to the stoichiometric ratio of the pigment phase;
s2) putting the weighed powder raw materials in the S1) into an agate mortar, and manually grinding to fully mix the raw materials;
s3) putting the mixed raw materials obtained in the step S2) into a tabletting mold, and tabletting and forming by using a tabletting machine;
and S4) putting the block pressed and formed in the # S3) into a corundum crucible, and sintering at high temperature in a box-type furnace according to a temperature rise curve to obtain the blue high near-infrared reflection blue inorganic pigment with a single blue phase.
8. The method according to claim 7, wherein the grinding time in S2) is 15-30min;
the diameter of the tabletting mold in the step S3) is 10-20mm, the pressure level of the pressing sample is 10-30MPa, and the pressure maintaining time is 1-5min.
9. The method according to claim 7, wherein the temperature-rise curve in S4) is:
firstly, heating to 1300-1500 ℃ according to the heating rate of 5-10 ℃/min, wherein the sintering time is 2-6h, and the sintering atmosphere is air;
then cooling according to the cooling rate of 5-10 ℃/min.
10. The method of claim 7, wherein the high nir reflecting blue inorganic pigment has a nir reflectance at 893nm of 80.5% to 90.7% and a nir reflectance at 1350nm of 66.3% to 85.8%.
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