CN114477266B - Method for improving near infrared reflectivity of yellow pigment - Google Patents
Method for improving near infrared reflectivity of yellow pigment Download PDFInfo
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- CN114477266B CN114477266B CN202210128870.1A CN202210128870A CN114477266B CN 114477266 B CN114477266 B CN 114477266B CN 202210128870 A CN202210128870 A CN 202210128870A CN 114477266 B CN114477266 B CN 114477266B
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- 239000001052 yellow pigment Substances 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000002310 reflectometry Methods 0.000 title abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 55
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 38
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 29
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 29
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 29
- 229910052751 metal Inorganic materials 0.000 claims abstract description 29
- 239000007864 aqueous solution Substances 0.000 claims abstract description 28
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 11
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 10
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 10
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000010304 firing Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 9
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 6
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims description 17
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical group Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 9
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical group CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 claims description 6
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical group Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000012805 post-processing Methods 0.000 claims description 2
- 238000009413 insulation Methods 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 18
- 238000001035 drying Methods 0.000 description 9
- 239000000049 pigment Substances 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 238000010532 solid phase synthesis reaction Methods 0.000 description 6
- 238000000227 grinding Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000012065 filter cake Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000001023 inorganic pigment Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical group [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 229910000410 antimony oxide Inorganic materials 0.000 description 1
- KKTCWAXMXADOBB-UHFFFAOYSA-N azanium;hydrogen carbonate;hydrate Chemical compound [NH4+].O.OC([O-])=O KKTCWAXMXADOBB-UHFFFAOYSA-N 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- IINACGXCEZNYTF-UHFFFAOYSA-K trichloroyttrium;hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Y+3] IINACGXCEZNYTF-UHFFFAOYSA-K 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
- C01F17/32—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 oxide or hydroxide being the only anion, e.g. NaCeO2 or MgxCayEuO
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses a method for improving near infrared reflectivity of a yellow pigment, which comprises the following chemical components in percentage by weight 2‑ x Y x Ce 2 O 7 Wherein x=0.2 to 1.0, the method comprising the steps of: (1) At 70-85 ℃, dropwise adding ammonium bicarbonate aqueous solution into a solution containing metal elements at a feeding speed of 35-65 mL/min for reaction to obtain a reaction solution, wherein the pH value of the reaction solution is controlled to be 6.6-7.2; (2) post-treating the reaction liquid to obtain a precursor; firing the precursor to obtain the yellow pigment; wherein the solution containing metal elements is an aqueous solution containing metal ions; the solution containing the metal elements is prepared from bismuth-containing inorganic salt, yttrium-containing inorganic salt and cerium-containing inorganic salt according to the mole ratio of Bi, Y and Ce in the yellow pigment. The method of the invention is beneficial to improving the near infrared reflectivity of the yellow pigment and improving the heat insulation performance of the yellow pigment.
Description
Technical Field
The invention relates to a method for improving near infrared reflectivity of a yellow pigment.
Background
Pigments are the main component that imparts color to the coating, and their reflectivity directly affects the thermal insulation properties of the coating. The near infrared reflectivity is an important index for judging the heat insulation performance of the pigment.
Research shows that the lanthanide inorganic pigment has excellent chemical stability and heat stability, and is a relatively promising optical material, such as yellow pigment Bi 2-x Y x Ce 2 O 7 (x=0.2 to 1.0). There are reports of obtaining the yellow pigment by subjecting the relevant metal ion oxide to multiple dry mixing, grinding, granulating, finally calcining the material at 1000 ℃ and conducting multiple grinding. However, the method relies on mechanical mixing, so that uneven raw material mixing is easy to cause, the purity of the product is not high, the particle size is uneven, and the near infrared reflectivity of the obtained yellow pigment is still to be improved. Therefore, how to increase the yellow pigment Bi 2-x Y x Ce 2 O 7 The near infrared reflectance of (x=0.2 to 1.0) is of great importance.
In addition, although the preparation methods of the inorganic pigments generally include a high-temperature solid-phase method, a liquid-phase precipitation method and a sol-gel method, what method is adopted and what specific conditions are adopted when different kinds of pigments are facedIt is not obvious that the thermal insulation properties of the pigment are better. For example, CN111039323A discloses a Bi doped with iron/terbium element 3 YO 6 The preparation method of the inorganic pigment comprises the steps of mixing and grinding oxides with acetone, drying and calcining to obtain a pigment product, wherein the near infrared reflectivity of the pigment product can reach 92.28 percent. CN101560343a discloses a method for preparing a heat-reflective heat-insulating inorganic material, which uses antimony oxide as a matrix and is doped with one or more elements of zinc, yttrium, cerium, tin, aluminum and bismuth. The preparation method adopts ethanol as a solvent, adopts sodium hydroxide solution as an alkaline solution, and adjusts the pH value. The near infrared reflectivity of the material obtained by the preparation method is more than 90 percent. The heat insulating inorganic material disclosed in the above patent document has a great difference from the present invention, and the preparation method thereof has little borrowable value.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for improving near infrared reflectance of a yellow pigment, which is capable of obtaining a yellow pigment having a high near infrared reflectance.
The invention achieves the above object by the following technical scheme.
The invention provides a method for improving near infrared reflectivity of yellow pigment, which comprises the following chemical components in percentage by weight 2-x Y x Ce 2 O 7 Wherein each element subscript represents a molar coefficient, x=0.2 to 1.0, the method comprising the steps of:
(1) At 70-85 ℃, dropwise adding ammonium bicarbonate aqueous solution into a solution containing metal elements at a feeding speed of 35-65 mL/min for reaction to obtain a reaction solution, wherein the pH value of the reaction solution is controlled to be 6.6-7.2;
(2) Post-processing the reaction liquid to obtain a precursor; firing the precursor to obtain the yellow pigment;
wherein the solution containing metal elements is an aqueous solution containing metal ions; the solution containing the metal elements is prepared from bismuth-containing inorganic salt, yttrium-containing inorganic salt and cerium-containing inorganic salt according to the mole ratio of Bi, Y and Ce in the yellow pigment.
According to the method of the present invention, preferably, the concentration of the ammonium bicarbonate aqueous solution is 1.5 to 2.5mol/L.
According to the method of the present invention, preferably, the concentration of the cerium-containing inorganic salt in the metal element-containing solution is 0.5 to 1.5mol/L based on the cerium element.
According to the method of the present invention, preferably, the ratio of the molar concentration of the ammonium bicarbonate aqueous solution to the molar concentration of the cerium-containing inorganic salt in the metal element-containing solution based on the cerium element is 1.8 to 2.7:1.
Preferably, the bismuth-containing inorganic salt is bismuth chloride, the yttrium-containing inorganic salt is yttrium chloride, and the cerium-containing inorganic salt is cerium chloride.
According to the method of the present invention, preferably, in the step (1), the reaction is continued for 20min to 3h after the completion of the dropwise addition.
According to the process of the present invention, preferably, in step (1), the reaction temperature is 75 to 85 ℃.
According to the method of the present invention, preferably, in the step (1), the feeding rate of the ammonium bicarbonate aqueous solution is 40-65 mL/min.
According to the method of the present invention, preferably, in the step (1), the pH of the reaction solution is 6.7 to 7.0.
According to the method of the present invention, preferably, in the step (2), the firing temperature is 900 to 1100 ℃ and the firing time is 1 to 8 hours.
Compared with the high-temperature solid phase method, the invention can ensure that the obtained yellow pigment has higher near infrared reflectivity and better heat insulation performance by dripping the ammonium bicarbonate water solution into the solution containing metal elements at a specific feeding speed and controlling the reaction temperature and the pH value within a specific range. In addition, the invention controls the ratio of the molar concentration of the ammonium bicarbonate aqueous solution and the molar concentration of the cerium-containing inorganic salt taking cerium element as the reference in the solution containing the metal element to react within a specific range, thereby being beneficial to improving the near infrared reflectivity of the yellow pigment. The near infrared reflectivity of the yellow pigment obtained by the method can reach 93.6 percent, which is obviously higher than that of the yellow pigment obtained by a high-temperature solid phase method (91.6 percent).
Drawings
FIG. 1 is an XRD pattern of the yellow pigment obtained in example 1.
Detailed Description
The present invention will be further described with reference to specific examples, but the scope of the present invention is not limited thereto.
The invention provides a method for improving near infrared reflectivity of a yellow pigment. The chemical composition of the yellow pigment is Bi 2-x Y x Ce 2 O 7 Wherein each element subscript represents a molar coefficient of from x=0.2 to 1.0, preferably from x=0.2 to 0.75, more preferably from x=0.25 to 0.5. According to one embodiment of the invention, the yellow pigment has a chemical composition of Bi 1.75 Y 0.25 Ce 2 O 7 。
The method of the invention comprises the following steps: (1) a feed reaction step; (2) a post-treatment step; (3) a firing step. The following is a detailed description.
< feeding reaction step >
And (3) dropwise adding the ammonium bicarbonate aqueous solution into the solution containing the metal elements for reaction to obtain a reaction solution. This is advantageous in that the resulting yellow pigment has a high near infrared reflectance. In the prior art, the yellow pigment is generally obtained by a high-temperature solid phase method. So far, the preparation of the yellow pigment Bi by adopting a liquid phase precipitation method has not been found 2-x Y x Ce 2 O 7 (x=0.2 to 1.0) and improves near infrared reflectance.
In the present invention, the molar concentration of the ammonium bicarbonate aqueous solution is 1.5 to 2.5mol/L, preferably 1.7 to 2.3mol/L, more preferably 1.8 to 2.2mol/L, still more preferably 1.9 to 2.1mol/L.
Through a great deal of researches and experiments, the charging speed of the ammonium bicarbonate aqueous solution is controlled within a specific range, which is favorable for obtaining yellow pigment with higher near infrared reflectivity. The feed rate of the ammonium bicarbonate aqueous solution is 35 to 65mL/min, preferably 40 to 60mL/min, more preferably 40 to 55mL/min, and still more preferably 45 to 50mL/min. This is probably because controlling the dropping speed can make the reaction mass more uniform and the particles of the resulting precursor more uniform.
In the present invention, the metal element-containing solution is an aqueous solution containing metal ions; the solution containing the metal elements is prepared from bismuth-containing inorganic salt, yttrium-containing inorganic salt and cerium-containing inorganic salt according to the mole ratio of Bi, Y and Ce in the yellow pigment.
In certain embodiments, the cerium-containing inorganic salt is cerium chloride. In other embodiments, the cerium-containing inorganic salt is cerium nitrate.
In certain embodiments, the yttrium-containing inorganic salt is yttrium chloride, preferably yttrium chloride hexahydrate. The bismuth-containing inorganic salt is bismuth chloride.
According to a preferred embodiment of the present invention, the cerium-containing inorganic salt is cerium chloride, the yttrium-containing inorganic salt is yttrium chloride, and the bismuth-containing inorganic salt is bismuth chloride.
When preparing the solution containing the metal element, the corresponding bismuth-containing inorganic salt, yttrium-containing inorganic salt and cerium-containing inorganic salt can be weighed according to the mole ratio of Bi, Y and Ce elements in the chemical composition of the yellow pigment and dissolved in water, so as to prepare the solution containing the metal element.
In some embodiments, the aqueous cerium chloride solution may be prepared first, and then the aqueous yttrium chloride solution and bismuth chloride may be added to the aqueous cerium chloride solution in a molar ratio of Bi, Y, and Ce elements of the yellow pigment chemical composition and mixed to obtain a metal element-containing solution.
In the solution containing a metal element of the present invention, the molar concentration of the cerium-containing inorganic salt is 0.5 to 1.5mol/L, preferably 0.7 to 1.5mol/L, more preferably 0.8 to 1.2mol/L, based on the cerium element.
In a preferred embodiment, the molar concentration of the aqueous ammonium bicarbonate to the molar concentration of the cerium-containing inorganic salt is in the range of 1.8 to 2.7:1, preferably 1.8 to 2.6:1, more preferably 2 to 2.5:1. This can be advantageous for improving the near infrared reflectance of the resulting yellow pigment.
In the invention, the dropping process is carried out at 70-85 ℃, namely, the reaction temperature is 70-85 ℃. Preferably, the dropping process is performed at 75 to 85 ℃, more preferably, the dropping process is performed at 77 to 82 ℃.
In the present invention, the reaction is continued for 20 minutes to 2 hours, preferably 0.5 to 1.5 hours, more preferably 0.5 to 1 hour after completion of the dropwise addition. The reaction temperature is kept at 70 to 85 ℃, preferably 75 to 85 ℃, more preferably 77 to 82 ℃.
In the present invention, the pH of the reaction solution is controlled to be 6.6 to 7.2, preferably 6.7 to 7.1, more preferably 6.7 to 7.0. This advantageously results in a higher near infrared reflectance of the resulting yellow pigment.
< post-treatment step >
And (3) carrying out post-treatment on the reaction liquid to obtain a precursor.
In the invention, the post-treatment comprises the steps of solid-liquid separation of reaction liquid to obtain a filter cake, and then drying to obtain a precursor.
The solid-liquid separation may be filtration or centrifugation, preferably filtration. During filtration, the solids may be rinsed with water to obtain a filter cake.
And drying the filter cake. The specific manner of drying is not particularly limited, and vacuum drying is preferable. The drying temperature may be 60 to 120 ℃, preferably 70 to 110 ℃, more preferably 70 to 100 ℃. The drying time may be 3 to 12 hours, preferably 3 to 10 hours, more preferably 4 to 10 hours. This is advantageous for obtaining yellow pigments having a higher near infrared reflectance.
< burning step >
And firing the precursor to obtain the yellow pigment. The chemical composition of the yellow pigment is Bi 2-x Y x Ce 2 O 7 Wherein x=0.2 to 1.0, preferably x=0.2 to 0.75.
The firing temperature is 900 to 1100 ℃, preferably 950 to 1100 ℃, more preferably 980 to 1050 ℃. The firing time is 1 to 8 hours, preferably 1.5 to 5 hours, more preferably 2 to 4 hours.
The near infrared reflectivity of the yellow pigment prepared by the invention can reach 93.6 percent.
< test method >
XRD: and (3) detecting by using a DX-27mini table type diffractometer.
Near infrared reflectance: detection was performed using a UH4150 UV-visible near infrared spectrophotometer.
Example 1
An aqueous cerium chloride solution was prepared at a concentration of 1mol/L. According to the yellow pigment Bi 1.75 Y 0.25 Ce 2 O 7 The molar ratio of Y, bi to Ce was obtained by adding an aqueous yttrium chloride solution (concentration: 2.63 mol/L) and bismuth chloride to a cerium chloride solution to obtain a metal element-containing solution (the molar concentration of cerium chloride based on cerium element, in the metal element-containing solution: 0.975 mol/L).
Preparing ammonium bicarbonate aqueous solution with concentration of 2mol/L.
At 80 ℃, dropwise adding an ammonium bicarbonate aqueous solution into the solution containing the metal element at a feeding speed of 45mL/min for reaction until the pH value of a reaction system is 6.7, stopping dropwise adding, and continuously stirring for reaction for 0.5h to obtain a reaction solution, wherein the pH value of the reaction solution is 6.7.
The reaction solution was filtered, and the solid was washed with water to obtain a cake. And (3) drying the filter cake in vacuum at 85 ℃ for 3 hours to obtain a precursor. The precursor is burned for 2 hours at 1000 ℃ to obtain the yellow pigment. XRD of the yellow pigment obtained is shown in FIG. 1, and the near infrared reflectance results are shown in Table 1.
Example 2
The only difference from example 1 is that the feed rate of the aqueous ammonium bicarbonate solution was 50mL/min. The near infrared reflectance results of the obtained yellow pigment are shown in Table 1.
Comparative examples 1 and 2
The difference from example 1 is that the feed rate of the aqueous ammonium bicarbonate solution is different. The specific parameters and the near infrared reflectance results of the obtained yellow pigment are shown in Table 1.
Comparative examples 3 to 4
The difference from example 1 is that the pH of the reaction solution is different. The specific parameters and the near infrared reflectance results of the obtained yellow pigment are shown in Table 1.
Comparative examples 5 to 6
The difference from example 1 is that the reaction temperature is different. The specific parameters and the near infrared reflectance results of the obtained yellow pigment are shown in Table 1.
Comparative examples 7 to 8
The difference from example 1 is only that the molar concentration of the ammonium bicarbonate aqueous solution is different from the molar concentration of the cerium-containing inorganic salt based on the cerium element (denoted as M) in the metal element-containing solution. In comparative example 7, the molar concentration of the ammonium bicarbonate aqueous solution was 1mol/L. In comparative example 8, the concentration of the ammonium bicarbonate aqueous solution was 3mol/L. The near infrared reflectance results of the obtained yellow pigment are shown in Table 1.
Comparative example 9
The only difference from example 1 is the manner of addition. The ammonium bicarbonate aqueous solution and the solution containing the metal element are added dropwise in parallel (i.e. simultaneously added into the reaction kettle). The near infrared reflectance results of the obtained yellow pigment are shown in Table 1.
Comparative example 10
The only difference from example 1 is that comparative example 10 uses ammonia instead of ammonium bicarbonate aqueous solution. The near infrared reflectance results of the obtained yellow pigment are shown in Table 1.
Comparative example 11
The difference from example 1 is that a yellow pigment is prepared by a high temperature solid phase method. I.e. according to the yellow pigment Bi 1.75 Y 0.25 Ce 2 O 7 The molar ratio of Bi, Y and Ce elements is called Bi with corresponding weight 2 O 3 、CeO 2 、Y 2 O 3 Mixing the oxides with acetone, grinding, and drying at 100deg.C; then, mixing with acetone repeatedly, grinding and drying three times to obtain powder. The powder was calcined at 1000℃for 6 hours to give a yellow pigment. The near infrared reflectance of the obtained pigment was 91.6%.
Table 1 process parameters and test results for examples and comparative examples
Note that: in Table 1, the feed rate of the aqueous ammonium bicarbonate solution is reported as V. The ratio of the molar concentration of the ammonium bicarbonate aqueous solution to the molar concentration of the cerium-containing inorganic salt in the metal element-containing solution based on the cerium element is denoted as M.
As is clear from the comparison of examples and comparative examples 1 and 2, the addition rate of the ammonium bicarbonate aqueous solution cannot be too high or too slow, and the addition rate needs to be controlled within a certain range to be beneficial to improving the near infrared reflectivity of the obtained yellow pigment.
As is clear from comparison of examples and comparative examples 3 and 4, the control of the pH of the reaction system and the reaction liquid within a specific range can make the near infrared reflectance of the obtained yellow pigment higher.
As is clear from comparison of examples and comparative examples 5 and 6, the reaction temperature at the time of dropwise addition needs to be controlled within a specific range, and the technical effect of the present invention cannot be achieved even if the temperature is too high or too low.
As is clear from comparison of examples and comparative examples 7 and 8, the magnitude of the ratio of the molar concentration of the ammonium bicarbonate aqueous solution to the molar concentration of the cerium-containing inorganic salt based on the cerium element in the metal element-containing solution has an unexpected effect on the near infrared reflectance of the resulting yellow pigment.
As is clear from the comparison between the examples and the comparative example 9, the feeding method of the present invention is more advantageous for improving the near infrared reflectance of the yellow pigment.
As can be seen from comparison of examples and comparative example 10, the near infrared reflectance of the yellow pigment obtained by using ammonium bicarbonate aqueous solution as the precipitant is greater than that of the pigment obtained by using ammonia water as the precipitant.
As is clear from the comparison between examples and comparative example 11, the yellow pigment obtained by the method of the present invention has higher near infrared reflectance and better heat insulating property than the high temperature solid phase method.
The present invention is not limited to the above-described embodiments, and any modifications, improvements, substitutions, and the like, which may occur to those skilled in the art, fall within the scope of the present invention without departing from the spirit of the invention.
Claims (7)
1. A method for improving near infrared reflectance of a yellow pigment, comprising:
the chemical composition of the yellow pigment is Bi 2-x Y x Ce 2 O 7 Wherein, each element subscript represents a molar coefficient and x=0.2 to 1.0;
the method comprises the following steps:
(1) Dropwise adding an ammonium bicarbonate aqueous solution into a solution containing metal elements at a feeding speed of 35-65 mL/min at 70-85 ℃ for reaction, and continuing to react for 20-3 h at 70-85 ℃ after the dropwise adding to obtain a reaction solution, wherein the pH value of the reaction solution is controlled to be 6.6-7.2;
(2) Post-processing the reaction liquid to obtain a precursor; firing the precursor at 900-1100 ℃ for 1-8 hours to obtain the yellow pigment;
wherein the solution containing metal elements is an aqueous solution containing metal ions; the solution containing the metal elements is prepared from bismuth-containing inorganic salt, yttrium-containing inorganic salt and cerium-containing inorganic salt according to the mole ratio of Bi, Y and Ce in the yellow pigment;
wherein the ratio of the molar concentration of the ammonium bicarbonate aqueous solution to the molar concentration of the cerium-containing inorganic salt in the solution containing the metal element based on the cerium element is 1.8-2.7:1.
2. The method according to claim 1, wherein the concentration of the aqueous ammonium bicarbonate solution is 1.5 to 2.5mol/L.
3. The method according to claim 2, wherein the concentration of the cerium-containing inorganic salt in the solution containing the metal element is 0.5 to 1.5mol/L based on the cerium element.
4. The method of claim 1, wherein the bismuth-containing inorganic salt is bismuth chloride, the yttrium-containing inorganic salt is yttrium chloride, and the cerium-containing inorganic salt is cerium chloride.
5. The process according to claim 1, wherein in step (1), the reaction temperature is 75 to 85 ℃.
6. The method according to claim 1, wherein in step (1), the feeding rate of the ammonium bicarbonate aqueous solution is 40-65 mL/min.
7. The method according to claim 1, wherein in the step (1), the pH of the reaction solution is 6.7 to 7.0.
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