CN116063079A - Rare earth cold pigment of molybdenum cerium acid and preparation method thereof - Google Patents
Rare earth cold pigment of molybdenum cerium acid and preparation method thereof Download PDFInfo
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 55
- 239000002253 acid Substances 0.000 title claims abstract description 51
- 239000000049 pigment Substances 0.000 title claims abstract description 49
- RQYSWULBRFINID-UHFFFAOYSA-N [Mo].[Ce] Chemical compound [Mo].[Ce] RQYSWULBRFINID-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title abstract description 20
- -1 rare earth nitrate Chemical class 0.000 claims abstract description 37
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 28
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 27
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 13
- 238000001704 evaporation Methods 0.000 claims abstract description 12
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 11
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 10
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 10
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 10
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 16
- 239000011240 wet gel Substances 0.000 claims description 14
- 230000035484 reaction time Effects 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 241000282414 Homo sapiens Species 0.000 abstract description 7
- 231100000053 low toxicity Toxicity 0.000 abstract description 5
- 231100000419 toxicity Toxicity 0.000 abstract description 3
- 230000001988 toxicity Effects 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 30
- 230000007797 corrosion Effects 0.000 description 26
- 238000005260 corrosion Methods 0.000 description 26
- 239000000919 ceramic Substances 0.000 description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 20
- 238000002310 reflectometry Methods 0.000 description 18
- 239000000243 solution Substances 0.000 description 17
- 238000005530 etching Methods 0.000 description 13
- 238000001514 detection method Methods 0.000 description 10
- 238000005265 energy consumption Methods 0.000 description 9
- XOFYZVNMUHMLCC-ZPOLXVRWSA-N prednisone Chemical compound O=C1C=C[C@]2(C)[C@H]3C(=O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 XOFYZVNMUHMLCC-ZPOLXVRWSA-N 0.000 description 9
- 238000000576 coating method Methods 0.000 description 8
- 238000004090 dissolution Methods 0.000 description 8
- IDBATCVUKYAUDT-UHFFFAOYSA-N [Ce].[La].[Mo] Chemical compound [Ce].[La].[Mo] IDBATCVUKYAUDT-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 description 5
- 229960002303 citric acid monohydrate Drugs 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 239000002270 dispersing agent Substances 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 5
- 238000000985 reflectance spectrum Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 229910021642 ultra pure water Inorganic materials 0.000 description 5
- 239000012498 ultrapure water Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 229960004106 citric acid Drugs 0.000 description 4
- CFYGEIAZMVFFDE-UHFFFAOYSA-N neodymium(3+);trinitrate Chemical compound [Nd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CFYGEIAZMVFFDE-UHFFFAOYSA-N 0.000 description 4
- YZDZYSPAJSPJQJ-UHFFFAOYSA-N samarium(3+);trinitrate Chemical compound [Sm+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YZDZYSPAJSPJQJ-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- PYWIBSWKZCVRAA-UHFFFAOYSA-N [Nd].[Sm].[La] Chemical compound [Nd].[Sm].[La] PYWIBSWKZCVRAA-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- QXDSNHQDQNPXCH-UHFFFAOYSA-N cerium lanthanum neodymium Chemical compound [La][Nd][Ce] QXDSNHQDQNPXCH-UHFFFAOYSA-N 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(3+);trinitrate Chemical compound [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 description 2
- 239000005431 greenhouse gas Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- LLZBVBSJCNUKLL-UHFFFAOYSA-N thulium(3+);trinitrate Chemical compound [Tm+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O LLZBVBSJCNUKLL-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- WCYXDPQRKFQCSQ-UHFFFAOYSA-N [Nd].[Sm] Chemical compound [Nd].[Sm] WCYXDPQRKFQCSQ-UHFFFAOYSA-N 0.000 description 1
- UOEPLZZWSQSTOS-UHFFFAOYSA-N [Tm].[Sm].[Eu] Chemical compound [Tm].[Sm].[Eu] UOEPLZZWSQSTOS-UHFFFAOYSA-N 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- LIJBQYBZQVLUTO-UHFFFAOYSA-N cerium;oxomolybdenum Chemical compound [Ce].[Mo]=O LIJBQYBZQVLUTO-UHFFFAOYSA-N 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- MOUPNEIJQCETIW-UHFFFAOYSA-N lead chromate Chemical compound [Pb+2].[O-][Cr]([O-])(=O)=O MOUPNEIJQCETIW-UHFFFAOYSA-N 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000001054 red pigment Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000001052 yellow pigment Substances 0.000 description 1
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/624—Sol-gel processing
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3256—Molybdenum oxides, molybdates or oxide forming salts thereof, e.g. cadmium molybdate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/443—Nitrates or nitrites
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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Abstract
The invention discloses a rare earth molybdenum cerium acid cold pigment and a preparation method thereof, relates to the technical field of near infrared inorganic cold pigment preparation, solves the problems that the existing cold pigment has certain toxicity and has certain harm to human bodies and environment, and has a chemical general formula of RE 2 MoCeO 7 The method comprises the steps of carrying out a first treatment on the surface of the Wherein RE is at least one element of La, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb, lu, sc, Y; the preparation method comprises the following steps: heating a mixed aqueous solution of ammonium molybdate, cerium nitrate, one or more than one rare earth nitrate, citric acid and ethylene glycol, reacting at a certain temperature to obtain a rare earth base molybdenum-cerium acid sol, sequentially evaporating and drying, and calcining the obtained xerogel to obtain the rare earth molybdenum-cerium acid cold pigment; the rare earth element has excellent photoelectric property and low toxicity, and solves the problem that the driven inorganic cold pigment has certain harm to human body and environment.
Description
Technical Field
The invention relates to the technical field of near infrared inorganic cold pigment preparation, in particular to a rare earth molybdenum cerium acid cold pigment and a preparation method thereof.
Background
To improve indoor thermal comfort, heating, ventilation and air conditioning (HVAC) systems are installed in large numbers and used at high frequencies inside buildings, and the widespread use of HVAC systems results in a large consumption of energy, resulting in a "net heating effect", which with the formation of a heat island effect will further exacerbate urban refrigeration energy consumption, and thus urban heat waves and harmful haze will also occur simultaneously. This phenomenon is repeated and repeated, which causes the consumption of energy and the aggravation of environmental pollution, seriously threatens the survival of human beings, restricts the economic development and destroys the ecological balance. It is estimated that global building energy consumption is about 40% of the total global energy consumption, wherein the energy consumption caused by HVAC systems is about 30% of the total global energy consumption, and the greenhouse gas emissions caused by HVAC systems are about one third of the total emissions, which, if not controlled, would be expected to be about 50% of the total emissions by building energy consumption by 2050. Thus, controlling building energy consumption is one of the effective means to reduce greenhouse gas emissions, with the most critical issue being reducing building insulation and heat dissipation energy consumption.
On the market, building thermal management materials are mainly applied to: transparent coatings, radiant coolers, and inorganic pigment coatings. For inorganic cold pigment coatings, infrared radiation is passed through the white coating while reflecting a substantial portion of the incident solar radiation. Therefore, white paint has been studied more, and the commonly used inorganic cold pigment is titanium dioxide (TiO 2 ) And silicon dioxide (SiO) 2 ) Both of which are provided withHas excellent whiteness and higher solar emissivity. Research shows that TiO is prepared on the surface of an aluminum substrate 2 +SiO 2 The coating can reflect 90.7% of solar radiation at maximum, wherein the infrared emissivity reaches 90.11%, and the surface temperature of the aluminum foil can be reduced by 5-8 ℃. In addition, the coating is made into a three-dimensional hollow spherical coating, and the effects of warming in winter and cooling in summer can be realized through the synergistic effect of a plurality of components. However, white paint is vulnerable to environmental pollution, and once the surface adheres to impurity particles, the infrared properties thereof are easily affected. The solar reflectance properties of conventional pigments can be greatly improved by using colorants having high solar reflectance properties instead of conventional pigments, and thus researchers have begun to seek color paints having excellent infrared properties. The inorganic cold pigment is a key for determining the heat insulation performance of the coating, and has high near infrared reflectivity, high coverage rate and excellent weather resistance, so that the inorganic cold pigment can be widely applied in the field of energy conservation and environmental protection, and a new strategy is provided for solving a series of problems such as urban heat island, energy consumption and the like.
The traditional inorganic cold pigment is composed of mixed oxides, and the material is required to have high near infrared/hemispherical emissivity and low heat conductivity. Rutile titanium dioxide, although highly reflective in the near infrared, does not meet the requirements of modern application settings and has poor stain resistance. Yellow and red pigments, by contrast, exhibit superior infrared properties.
The yellow cold pigments commonly used at present comprise lead chromate, cadmium yellow, chrome titanate yellow and the like, but the cold pigments have certain toxicity and cause certain harm to human bodies and the environment. Meanwhile, in response to the sustainable development and the trend toward the dual-carbon wood standard in the chemical industry, development of a novel cold pigment with high near infrared reflection and no toxicity is urgent.
Disclosure of Invention
The invention aims to solve the problems that the existing cold pigment has certain toxicity and has certain harm to human bodies and the environment, and provides a rare earth molybdenum cerium acid cold pigment and a preparation method thereof.
The invention adopts the following technical scheme for realizing the purposes:
a rare earth molybdate cold pigment has a chemical formula of RE 2 MoCeO 7 The method comprises the steps of carrying out a first treatment on the surface of the Wherein RE is at least one element of La, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb, lu, sc, Y.
Further, RE consists of two elements, RE is A a B b A=b, and a+b=1, wherein A, B is selected from any one element in La, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb, lu, sc, Y, respectively, and A, B is a different element.
Further, RE is composed of three elements, RE is A a B b C c A=b=c, and a+b+c=1, wherein A, B, C is selected from any one element in La, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb, lu, sc, Y, respectively, and A, B, C is a different element.
Further, RE consists of four elements, RE is A a B b C c D d A=b=c=d, and a+b+c+d=1, wherein A, B, C, D is selected from any one element in La, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb, lu, sc, Y, and A, B, C, D is a different element.
Further, RE consists of four elements, RE is A a B b C c D d E e A=b=c=d=e, and a+b+c+d+e=1, wherein A, B, C, D, E is selected from any one element in La, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb, lu, sc, Y, and A, B, C, D, E is a different element, respectively.
The rare earth element used in the application has excellent photoelectric property and low toxicity, and solves the problem that the driven inorganic cold pigment has certain harm to human bodies and the environment. In addition, compared with the traditional ceramic material, the high-entropy material has thermodynamic high-entropy effect, structural lattice distortion effect, kinetic delayed diffusion effect and performance cocktail effect, so that rare earth elements with different characteristic peaks under infrared are combined by utilizing a high-entropy means, and the obtained rare earth molybdate cold pigment has the characteristics of high near infrared reflectivity and capability of selectively reflecting infrared bands.
In order to achieve the above purpose, the present application further provides a preparation method of the rare earth molybdenum cerium acid cold pigment, which comprises the following steps:
step 1: heating a mixed aqueous solution of ammonium molybdate, cerium nitrate, one or more than one rare earth nitrate, citric acid and ethylene glycol, and reacting at a certain temperature to obtain rare earth molybdenum-cerium acid-based sol; wherein the rare earth nitrate has a chemical formula of RE (NO) 3 ) 3 ；
Step 2: evaporating the rare earth molybdenum-cerium acid-based sol obtained in the step 1 to obtain rare earth molybdenum-cerium acid wet gel, and drying the rare earth molybdenum-cerium acid wet gel to obtain xerogel;
step 3: calcining the xerogel obtained in the step 2 to obtain the rare earth molybdenum cerium acid powder material, namely the rare earth molybdenum cerium acid cold pigment.
Further, when two or more rare earth nitrates are used in step 1, the molar amount of rare earth element contained in each rare earth nitrate is the same.
Further, mo in ammonium molybdate in step 1 6+ Ce in cerium nitrate 3+ RE in rare earth nitrate 3+ The molar ratio of (2) is 1:1:2; mo (Mo) 6+ 、Ce 3+ 、RE 3+ In terms of ME 3+ Total (S) Representation, ME 3+ Total (S) The molar ratio of the citric acid to the citric acid is 1: (1.0-2); the mass ratio of the citric acid to the glycol is 1: (1.0-2.0).
Further, the heating temperature in the step 1 is 70-90 ℃, the reaction time is 2-4 hours, and stirring is kept under the heating condition, wherein the stirring speed is 200-500rpm.
Further, the evaporating temperature in the step 2 is 80-110 ℃, and the reaction time is 2-4h; the drying temperature is 100-130 ℃, and the reaction time is 3-6 hours; stopping stirring during evaporation; the calcination temperature in the step 3 is 1100-1400 ℃ and the reaction time is 4-6h.
The preparation method of the rare earth molybdenum cerium acid cold pigment by adopting the sol-gel method has the advantages of simple preparation process, simple flow, controllable operation conditions, high purity, potential for large-scale industrial production, low toxicity and high chemical stability compared with the traditional cold pigment.
The beneficial effects of the invention are as follows:
(1) The rare earth element adopted by the method has excellent photoelectric property and low toxicity, and solves the problem that the driven inorganic cold pigment has certain harm to human bodies and the environment;
(2) The application combines rare earth elements with different characteristic peaks under infrared by utilizing a high entropy means, and the obtained rare earth cold pigment of the molybdenum cerium acid has the characteristics of high near infrared reflectivity and capability of selectively reflecting infrared wave bands;
(3) The preparation method of the rare earth molybdenum cerium acid cold pigment by adopting the sol-gel method has the advantages of simple preparation process, simple flow, controllable operation conditions, high purity, potential for large-scale industrial production, low toxicity and high chemical stability compared with the traditional cold pigment.
Drawings
FIG. 1 is an XRD pattern of rare earth molybdenum cerium acid prepared in examples 1-5 of the present invention;
FIG. 2 is a near infrared reflectance spectrum of lanthanum molybdenum cerium acid prepared in example 1 of the present invention;
FIG. 3 is a near infrared reflectance spectrum of lanthanum neodymium cerium molybdenum oxide prepared in example 2 of the present invention;
FIG. 4 is a near infrared reflectance spectrum of lanthanum neodymium samarium molybdenum cerium acid prepared in example 3 of the present invention;
FIG. 5 is a near infrared reflectance spectrum of lanthanum neodymium samarium europium molybdenum cerium acid prepared in example 4 of the present invention;
fig. 6 is a near infrared reflectance spectrum of lanthanum neodymium samarium europium thulium molybdenum cerium acid prepared in example 5 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
Example 1
The embodiment provides a preparation method of a lanthanum cerium molybdenum acid cold pigment, which comprises the following specific steps:
step 1: respectively weighing 0.004mol of ammonium molybdate and cerium nitrate, 0.008mol of lanthanum nitrate and 0.024mol of citric acid monohydrate, placing into a beaker, adding 100ml of ultrapure water for dissolution, and adding 7.57g of ethylene glycol serving as a dispersing agent after complete dissolution; the prepared solution reacts for 4 hours at the temperature of 70 ℃ and the stirring speed of 300rpm to form sol;
step 2: stopping stirring, and evaporating the sol at 90 ℃ for 4 hours to form wet gel; drying the wet gel at 110 ℃ for 6 hours to obtain xerogel;
step 3: calcining the xerogel at 1100 ℃ for 6 hours to obtain lanthanum molybdenum cerium (La) 2 MoCeO 7 ) Ceramic powder.
And (3) performance detection: lanthanum molybdenum cerium (La) 2 MoCeO 7 ) The ceramic powder was detected by an X-ray diffractometer, and the XRD pattern obtained by the detection is shown in FIG. 1, and the peaks are sharp and free from burrs, indicating that the obtained lanthanum molybdenum cerium (La) 2 MoCeO 7 ) The ceramic powder has complete crystal form. The reflectivity of the near infrared band of 700-2500nm is shown in figure 2, the average reflectivity is 110.21%, and the material has excellent near infrared reflectivity.
Acid-base corrosion experiment: 3 groups of lanthanum cerium molybdenum (La) 2 MoCeO 7 ) The ceramic powder is respectively soaked in 5% hydrochloric acid, 5% sulfuric acid and 5% sodium hydroxide solution, kept for 24 hours, taken out and dried. At the same time according to the formula Δe= [ (Δl:) 2 +(Δa*) 2 +(Δb*) 2 ] 1/2 Calculating a chromaticity difference, wherein delta E is less than 6, and the color of the material is considered to have no obvious deviation, wherein delta E represents the chromaticity difference after acid-base corrosion; Δl represents the degree of color deviation after acid-base corrosion; Δa represents the red-green difference after acid-base corrosion; Δb represents the yellow-blue difference after acid-base corrosion.
Experimental results: the chromaticity difference is shown in table 1 below.
TABLE 1
As can be seen from the test data in Table 1, the difference in chromaticity after etching with 5% hydrochloric acid, 5% sulfuric acid, 5% sodium hydroxide solution was less than 6, which indicates that the material had no significant deviation in color before and after etching, and further indicates that lanthanum molybdenum cerium (La 2 MoCeO 7 ) The ceramic powder has excellent chemical stability.
Example 2
The embodiment provides a preparation method of a lanthanum neodymium cerium molybdenum oxide cold pigment, which comprises the following specific steps:
step 1: respectively weighing 0.004mol of ammonium molybdate and cerium nitrate, 0.004mol of lanthanum nitrate, neodymium nitrate and samarium nitrate, and 0.024mol of citric acid monohydrate into a beaker, adding 100ml of ultrapure water for dissolution, and adding 5.04g of ethylene glycol serving as a dispersing agent after complete dissolution; the prepared solution reacts for 3 hours at the temperature of 80 ℃ and the stirring speed of 500rpm to form sol;
step 2: stopping stirring, and evaporating the sol at 100 ℃ for 3 hours to form wet gel; drying the wet gel at 110 ℃ for 5 hours to obtain xerogel;
step 3: calcining the xerogel at 1200 ℃ for 5 hours to obtain the lanthanum neodymium molybdenum cerium acid LaNdMoCeO 7 Ceramic powder.
And (3) performance detection: lanthanum neodymium cerium molybdate LaNdMoCeO prepared by the method of example 2 7 The ceramic powder is detected by an X-ray diffractometer, the XRD pattern obtained by the detection is shown in figure 1, and the peaks are sharp and have no burrs, which shows that the obtained lanthanum neodymium molybdenum cerium acid LaNdMoCeO 7 The ceramic powder has complete crystal form. The reflectivity of the near infrared band of 700-2500nm is shown in figure 3, the average reflectivity is 103.30%, and the material has excellent near infrared reflectivity.
Acid-base corrosion experiment: taking 3 groups of lanthanum neodymium cerium molybdenum oxide LaNdMoCeO prepared in example 2 7 The ceramic powder is respectively soaked in 5% hydrochloric acid, 5% sulfuric acid and 5% sodium hydroxide solution, kept for 24 hours, taken out and dried,and the quality before and after corrosion was compared. At the same time according to the formula Δe= [ (Δl:) 2 +(Δa*) 2 +(Δb*) 2 ] 1/2 Calculating a chromaticity difference, wherein delta E is less than 6, and the color of the material is considered to have no obvious deviation, wherein delta E represents the chromaticity difference after acid-base corrosion; Δl represents the degree of color deviation after acid-base corrosion; Δa represents the red-green difference after acid-base corrosion; Δb represents the yellow-blue difference after acid-base corrosion.
Experimental results: the chromaticity difference is shown in table 2 below.
TABLE 2
As can be seen from the test data in Table 2, the difference in chromaticity after etching with 5% hydrochloric acid, 5% sulfuric acid, and 5% sodium hydroxide solution was less than 6, which indicates that the material had no significant deviation in color before and after etching, and further indicates that the lanthanum neodymium molybdenum cerium acid LaNdMoCeO prepared by the preparation method of example 2 7 The ceramic powder has excellent chemical stability.
Example 3
The embodiment provides a preparation method of a lanthanum neodymium cerium acid samarium cold pigment, which comprises the following specific steps:
step 1: respectively weighing 0.004mol of ammonium molybdate and cerium nitrate, 0.0026mol of lanthanum nitrate, neodymium nitrate and samarium nitrate, and 0.0192mol of citric acid monohydrate into a beaker, adding 100ml of ultrapure water for dissolution, and adding 4.84g of ethylene glycol serving as a dispersing agent after complete dissolution; the prepared solution reacts for 3 hours at the temperature of 80 ℃ and the stirring speed of 400rpm to form sol;
step 2: stopping stirring, and evaporating the sol at 100 ℃ for 3 hours to form wet gel; drying the wet gel at 120 ℃ for 5 hours to obtain xerogel;
step 3: calcining the xerogel at 1200deg.C for 5h to obtain lanthanum neodymium samarium (La) 1/3 Nd 1/ 3 Sm 1/3 ) 2 MoCeO 7 Ceramic powder.
And (3) performance detection: will employ example 3Lanthanum neodymium samarium (La) molybdenum cerium acid prepared by the method 1/3 Nd 1/3 Sm 1/3 ) 2 MoCeO 7 The ceramic powder is detected by an X-ray diffractometer, the XRD pattern obtained by the detection is shown in figure 1, and the peaks are sharp and have no burrs, which shows that the obtained lanthanum neodymium samarium (La) 1/3 Nd 1/3 Sm 1/3 ) 2 MoCeO 7 The ceramic powder has complete crystal form. The reflectivity of the near infrared band of 700-2500nm is shown in figure 4, the average reflectivity is 96.40%, and the material has excellent near infrared reflectivity.
Acid-base corrosion experiment: 3 groups of lanthanum neodymium cerium molybdenum cerium oxide samarium (La) prepared in example 3 were taken 1/3 Nd 1/3 Sm 1/3 ) 2 MoCeO 7 The ceramic powder was immersed in 5% hydrochloric acid, 5% sulfuric acid, and 5% sodium hydroxide solution, respectively, and kept for 24 hours, and dried after taking out, and the quality was compared before and after etching. At the same time according to the formula Δe= [ (Δl:) 2 +(Δa*) 2 +(Δb*) 2 ] 1/2 Calculating a chromaticity difference, wherein delta E is less than 6, and the color of the material is considered to have no obvious deviation, wherein delta E represents the chromaticity difference after acid-base corrosion; Δl represents the degree of color deviation after acid-base corrosion; Δa represents the red-green difference after acid-base corrosion; Δb represents the yellow-blue difference after acid-base corrosion.
Experimental results: the chromaticity difference is shown in table 3 below.
TABLE 3 Table 3
As can be seen from the test data in Table 3, the difference in chromaticity after etching with 5% hydrochloric acid, 5% sulfuric acid, 5% sodium hydroxide solution was less than 6, which indicates that the material had no significant deviation in color before and after etching, and further indicates that lanthanum neodymium samarium molybdenum cerium oxide (La 1/3 Nd 1/3 Sm 1/3 ) 2 MoCeO 7 The ceramic powder has excellent chemical stability.
Example 4
The embodiment provides a preparation method of a molybdenum cerium acid lanthanum neodymium samarium europium thulium cold pigment, which comprises the following specific steps:
step 1: respectively weighing 0.004mol of ammonium molybdate and cerium nitrate, 0.002mol of lanthanum nitrate, neodymium nitrate, samarium nitrate, europium nitrate and thulium nitrate and 0.024mol of citric acid monohydrate, placing into a beaker, adding 100ml of ultrapure water for dissolution, and adding 10.09g of ethylene glycol serving as a dispersing agent to be completely dissolved; reacting the prepared solution for 2 hours at 90 ℃ and a stirring speed of 500rpm to form sol;
step 2: stopping stirring, and evaporating the sol at 100 ℃ for 2 hours to form wet gel; drying the wet gel at 120 ℃ for 3 hours to obtain xerogel;
step 3: calcining the xerogel at 1400 ℃ for 4 hours to obtain the lanthanum neodymium samarium europium (La) 0.25 Nd 0.25 Sm 0.25 Eu 0.25 ) 2 MoCeO 7 Ceramic powder.
And (3) performance detection: the lanthanum neodymium samarium europium molybdenum cerium acid (La) prepared by the method of example 4 0.25 Nd 0.25 Sm 0.25 Eu 0.25 ) 2 MoCeO 7 The ceramic powder is detected by an X-ray diffractometer, the XRD chart obtained by the detection is shown in figure 1, and the peaks are sharp and have no burrs, which shows that the obtained molybdenum cerium acid lanthanum neodymium samarium europium thulium (La) 0.2 Nd 0.2 Sm 0.2 Eu 0.2 Tm 0.2 ) 2 MoCeO 7 The ceramic powder has complete crystal form. The reflectivity of the near infrared band of 700-2500nm is shown in figure 5, the average reflectivity is 91.26%, and the material has excellent near infrared reflectivity.
Acid-base corrosion experiment: 3 groups of lanthanum neodymium samarium europium (La) cerium molybdenum oxide prepared in example 4 were taken 0.25 Nd 0.25 Sm 0.25 Eu 0.25 ) 2 MoCeO 7 The ceramic powder was immersed in 5% hydrochloric acid, 5% sulfuric acid, and 5% sodium hydroxide solution, respectively, and kept for 24 hours, and dried after taking out, and the quality was compared before and after etching. At the same time according to the formula Δe= [ (Δl:) 2 +(Δa*) 2 +(Δb*) 2 ] 1/2 Calculating a chromaticity difference, wherein delta E is less than 6, and the color of the material is considered to have no obvious deviation, whereinΔe represents the chromaticity difference after acid-base corrosion; Δl represents the degree of color deviation after acid-base corrosion; Δa represents the red-green difference after acid-base corrosion; Δb represents the yellow-blue difference after acid-base corrosion.
Experimental results: the chromaticity difference is shown in table 4 below.
TABLE 4 Table 4
As can be seen from the test data in Table 4, the difference in chromaticity after etching with 5% hydrochloric acid, 5% sulfuric acid, 5% sodium hydroxide solution was less than 6, which indicates that the material had no significant deviation in color before and after etching, and further indicates that lanthanum neodymium samarium europium molybdenum cerium oxide (La 0.25 Nd 0.25 Sm 0.25 Eu 0.25 ) 2 MoCeO 7 The ceramic powder has excellent chemical stability.
Example 5
The embodiment provides a preparation method of a molybdenum cerium acid lanthanum neodymium samarium europium thulium cold pigment, which comprises the following specific steps:
step 1: respectively weighing 0.004mol of ammonium molybdate and cerium nitrate, 0.0016mol of lanthanum nitrate, neodymium nitrate, samarium nitrate, europium nitrate and thulium nitrate and 0.0288mol of citric acid monohydrate, placing into a beaker, adding 100ml of ultrapure water for dissolution, and adding 10.89g of ethylene glycol serving as a dispersing agent to be completely dissolved; reacting the prepared solution for 2 hours at 90 ℃ and a stirring speed of 500rpm to form sol;
step 2: stopping stirring, and evaporating the sol at 1100 ℃ for 2 hours to form wet gel; drying the wet gel at 130 ℃ for 3 hours to obtain xerogel;
step 3: calcining the xerogel at 1400 ℃ for 4 hours to obtain the lanthanum neodymium samarium europium (La) 0.2 Nd 0.2 Sm 0.2 Eu 0.2 Tm 0.2 ) 2 MoCeO 7 Ceramic powder.
And (3) performance detection: the lanthanum neodymium samarium europium (La) molybdenum cerium acid prepared by the method of example 5 0.2 Nd 0.2 Sm 0.2 Eu 0.2 Tm 0.2 ) 2 MoCeO 7 The ceramic powder is detected by an X-ray diffractometer, the XRD chart obtained by the detection is shown in figure 1, and the peaks are sharp and have no burrs, which shows that the obtained molybdenum cerium acid lanthanum neodymium samarium europium thulium (La) 0.2 Nd 0.2 Sm 0.2 Eu 0.2 Tm 0.2 ) 2 MoCeO 7 The ceramic powder has complete crystal form. The reflectivity of the near infrared band of 700-2500nm is shown in figure 6, the average reflectivity is 86.13%, and the material has excellent near infrared reflectivity.
Acid-base corrosion experiment: 3 groups of lanthanum neodymium cerium molybdenum cerium acid samarium europium thulium (La) prepared in example 5 were taken 0.2 Nd 0.2 Sm 0.2 Eu 0.2 Tm 0.2 ) 2 MoCeO 7 The ceramic powder was immersed in 5% hydrochloric acid, 5% sulfuric acid, and 5% sodium hydroxide solution, respectively, and kept for 24 hours, and dried after taking out, and the quality was compared before and after etching. At the same time according to the formula Δe= [ (Δl:) 2 +(Δa*) 2 +(Δb*) 2 ] 1/2 Calculating a chromaticity difference, wherein delta E is less than 6, and the color of the material is considered to have no obvious deviation, wherein delta E represents the chromaticity difference after acid-base corrosion; Δl represents the degree of color deviation after acid-base corrosion; Δa represents the red-green difference after acid-base corrosion; Δb represents the yellow-blue difference after acid-base corrosion.
Experimental results: the chromaticity difference is shown in table 5 below.
TABLE 5
As can be seen from the test data in Table 5, the difference in chromaticity after etching with 5% hydrochloric acid, 5% sulfuric acid, 5% sodium hydroxide solution was less than 6, which indicates that the material had no significant deviation in color before and after etching, and further indicates that the lanthanum neodymium samarium europium molybdenum (La) was prepared by the preparation method of example 5 0.2 Nd 0.2 Sm 0.2 Eu 0.2 Tm 0.2 ) 2 MoCeO 7 The ceramic powder has excellent chemical stability.
Claims (10)
1. A rare earth molybdenum cerium acid cold pigment is characterized in that the chemical general formula of the rare earth molybdenum cerium acid cold pigment is RE 2 MoCeO 7 The method comprises the steps of carrying out a first treatment on the surface of the Wherein RE is at least one element of La, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb, lu, sc, Y.
2. The rare earth molybdenum cerium acid cold pigment according to claim 1, wherein RE is composed of two elements, RE being a a B b A=b, and a+b=1, wherein A, B is selected from any one element in La, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb, lu, sc, Y, respectively, and A, B is a different element.
3. The rare earth molybdenum cerium acid cold pigment according to claim 1, wherein RE is composed of three elements, RE being a a B b C c A=b=c, and a+b+c=1, wherein A, B, C is selected from any one element in La, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb, lu, sc, Y, respectively, and A, B, C is a different element.
4. The rare earth molybdenum cerium acid cold pigment according to claim 1, wherein RE is composed of four elements, RE being a a B b C c D d A=b=c=d, and a+b+c+d=1, wherein A, B, C, D is selected from any one element in La, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb, lu, sc, Y, and A, B, C, D is a different element.
5. The rare earth molybdenum cerium acid cold pigment according to claim 1, wherein RE is composed of four elements, RE being a a B b C c D d E e A=b=c=d=e, and a+b+c+d+e=1, wherein A, B, C, D, E is selected from any one element in La, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb, lu, sc, Y, and A, B, C, D, E is a different element.
6. A method for preparing a rare earth molybdenum cerium acid cold pigment according to any one of claims 1 to 5, comprising the steps of:
step 1: heating a mixed aqueous solution of ammonium molybdate, cerium nitrate, one or more than one rare earth nitrate, citric acid and ethylene glycol, and reacting at a certain temperature to obtain rare earth molybdenum-cerium acid-based sol; wherein the rare earth nitrate has a chemical formula of RE (NO) 3 ) 3 ；
Step 2: evaporating the rare earth molybdenum-cerium acid-based sol obtained in the step 1 to obtain rare earth molybdenum-cerium acid wet gel, and drying the rare earth molybdenum-cerium acid wet gel to obtain xerogel;
step 3: calcining the xerogel obtained in the step 2 to obtain the rare earth molybdenum cerium acid powder material, namely the rare earth molybdenum cerium acid cold pigment.
7. The method for preparing a rare earth molybdenum cerium acid cold pigment according to claim 6, wherein when two or more rare earth nitrates are used in step 1, the molar amount of rare earth elements contained in each rare earth nitrate is the same.
8. The method for preparing a rare earth molybdate cold pigment according to claim 6, wherein Mo in the ammonium molybdate in the step 1 6+ Ce in cerium nitrate 3+ RE in rare earth nitrate 3+ The molar ratio of (2) is 1:1:2; mo (Mo) 6+ 、Ce 3+ 、RE 3+ In terms of ME 3+ Total (S) Representation, ME 3+ Total (S) The molar ratio of the citric acid to the citric acid is 1: (1.0-2); the mass ratio of the citric acid to the glycol is 1: (1.0-2.0).
9. The method for preparing a rare earth molybdenum cerium acid cold pigment according to claim 6, wherein the heating temperature in the step 1 is 70-90 ℃, the reaction time is 2-4 hours, and stirring is maintained under the heating condition at the same time, and the stirring speed is 200-500rpm.
10. The method for preparing a rare earth molybdenum cerium acid cold pigment according to claim 6, wherein the evaporating temperature in the step 2 is 80-110 ℃ and the reaction time is 2-4h; the drying temperature is 100-130 ℃, and the reaction time is 3-6 hours; stopping stirring during evaporation; the calcination temperature in the step 3 is 1100-1400 ℃ and the reaction time is 4-6h.
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