CN102688732A - Universal preparation method for rare earth oxide nanometer porous aerogel with high specific surface area - Google Patents
Universal preparation method for rare earth oxide nanometer porous aerogel with high specific surface area Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation of porous materials with high specific surface areas, and particularly relates to a universal preparation method for rare earth oxide nanometer porous aerogel with high specific surface area. The universal preparation method has the advantages that an inorganic dispersion sol-gel method is adopted, cheap rare earth element chloride solution is used as a precursor, various substances are used as complex agents, epoxide is used as a gel accelerator, a sol-gel process is combined with a drying process, and various rare earth oxide aerogel materials with high specific surface areas are prepared. The universal preparation method has the advantages that applicability is high, raw materials are cheap and are obtained easily, a reaction process is simple, total cost is low, and the like, the obtained materials are of nanoscale multi-stage micro-nano structures, the specific surface area of each material can be higher than 200m<2>/g, and the materials are widely applied to fields of high-performance fluorescent powder, metallurgical addition agents, catalysts, high-temperature superconductors, solid laser devices, high-temperature thermoelectric systems, glass and ceramic additives and the like.
Description
Technical field
The invention belongs to high specific surface area porous technical field of material, be specifically related to a kind of general preparation method of high-specific surface area nanometer rare earth oxide porous aerogel.
Background technology
The lanthanide series that rare earth element refers to III B family in the periodic table of elements adds the general name of 17 kinds of elements such as scandium and yttrium.Wherein, the nature difference of scandium and other rare earth element is bigger, and promethium is an artificial radioactive element, does not all study in this patent and protects.Rare earth oxide is widely used in directions such as high-performance fluorescent material, metallurgical addition agent, catalyst, high-temperature superconductor, Solid State Laser, high temperature thermoelectricity and glass ceramics additives.Specific area is one of important parameter of weighing the active size of solid material; The rare earth oxide material of high-specific surface area all has obvious effects at aspect of performances such as improving catalysis, luminous, additive mixing uniformity, is the focus direction of present rare earth based functional material research.
Usually RE oxide powder is that method preparation through the compound powder pyrolytic gets, and its specific area is only at 2-4 m
2About/g.In patent of invention " large specific surface area earth-rare oxides and preparation method thereof " (ZL 96116316.X), introduced employing coprecipitation or mixing method and prepared and contain the hydrazine rare-earth oxalate, and prepared specific area up to 5-50 m through the method for thermal decomposition
2The multiple RE oxide powder of/g.
Adopting the aeroge of Prepared by Sol Gel Method is a kind of the gathering each other by nanometer scale ultrafine dust or high-polymer molecular to constitute the nanoporous network; And in hole, be full of a kind of high dispersive solid-state material of gaseous state decentralized medium; Its porosity can reach 80 ~ 99.8%; Generally between 1-100nm, specific area can be up to 100-3000 m for bore hole size
2/ g.Therefore; Aerogel material has particular performances; Low like Young's modulus and thermal conductivity, apparent density is little, refractive index is little and specific area is high, can be widely used in particle detector, heat insulation skylight, high-velocity particles protection and catch, aspects such as catalyst and catalyst carrier, luminous, high dielectric constant material.
The characteristics that aeroge has active high (specific area is high) and stability high (the multistage fractal nano porous network structure that connects each other) concurrently are very suitable for high-specific surface area rare earth oxide material.Yet, prepare aeroge usually and need adopt metal alkoxide to realize gelation (traditional sol-gal process) as presoma, adjusting pH value.Yet the alkoxide of rare earth element costs an arm and a leg even extremely is difficult to and obtains, and is not suitable for suitability for industrialized production and application.Seminar such as the A. E. Gash of the U.S. and L. J. Hope-Weeks and domestic Gan Lihua, Zhang Lin, appoint big waves and applicant seminar etc. to report the new technology that adopts inorganic salt solution and the multiple aeroge of organic epoxide prepared in reaction, expanded the preparation scope (epoxides method) of aeroge.Employing polyacrylic acid such as applicant Zhou Bin, Du Ai are dispersant and template; The coupling collar conventional ceramic technique; Solved the preparation problem of many families multicycle oxide-base aerogel material; Further expanded aeroge the preparation scope (" preparation method of transition metal base aeroge, transition metal oxide silica aerogel, composite transition metal oxide silica aerogel ", ZL200810033022.2).
Yet high-specific surface area rare earth oxide aeroge has bigger difficult point at aspects such as presoma selection, mouldability raising and micro-structural regulation and control, makes it to be different from the middle and high Z element of common trivalent, is difficult to directly adopt method for preparing.It is that presoma, epoxides are that the method for gel promoter has prepared multiple rare earth oxide aeroge that this patent adopts complexing agent restriction rare earth oxide colloid nucleation and growth (improve mouldability and also regulate and control micro-structural) combination inorganic salts.The method that the method that going back Shang Weijian at present has other document and patent report to adopt complexing agent to be constrained to nucleus growth is come synthesizing high specific surface area rare earth oxide aeroge.
Summary of the invention
The object of the present invention is to provide the general preparation method of a kind of applied widely, with low cost, reaction time of short, the high-specific surface area nanometer rare earth oxide porous aerogel that maybe industry amplifies.Its basic ideas are to combine the method for the sol-gel process (inorganic salts are that presoma, epoxides are gel promoter) of low reaction speed to realize that preparation, mouldability to the rare earth oxide aeroge improve and the micro-structural regulation and control through complexing agent restriction rare earth oxide colloid nucleation and growth (improve mouldability and regulate and control micro-structural).Obviously, adopt the thinking of similar complexing agent restriction nucleation and growth or adopt the mode of relevant mixed solvent to prepare the unit or the multielement rare earth oxide aeroge also belongs to protection scope of the present invention.Particular content is following:
The present invention proposes a kind of general preparation method of high-specific surface area nanometer rare earth oxide porous aerogel, adopt inorganic dispersion sol-gal process, concrete steps are following:
(1) the rare earth element chloride is dissolved in mixed solution that organic solvent and water forms or directly soluble in water, is mixed with the rare earth element chloride solution;
(2) in the solution of step (1) gained, add complexing agent and epoxides successively, stir, obtain gel after leaving standstill; Wherein, the adding proportion of chloride, organic solvent, water, complexing agent, epoxides is 6mmol:0 ~ 60ml:0.5 ~ 30ml:0-5ml:1-10ml;
(3) the aging at normal temperatures back of step (2) gained gel is dry, promptly obtain required rare earth oxide aerogel material.
Among the present invention, the rare earth element chloride described in the step (1) is any one or more than one the mixture in lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu) or yttrium (Y) chloride.
Among the present invention, the organic solvent described in step (1) and the step (2) is in the materials such as methyl alcohol, ethanol, acetone or acetonitrile any.
Among the present invention, the complexing agent described in the step (2) is that acetate, acetylacetone,2,4-pentanedione or polyacrylic acid etc. have in the material of coordination ability any.
Among the present invention, the epoxides described in the step (2) is that expoxy propane, oxirane or epoxychloropropane etc. have in the compound of epoxide group any.
Among the present invention, drying means described in the step (3) be in the modes such as supercritical fluid drying, freeze drying, heat de-airing drying or normal pressure air dry any.
The rare earth oxide aeroge of the present invention's preparation has high-specific surface area and multistage fractal nanoporous network structure, and is higher in constitutionally stable while activity, successfully solved the general preparation difficult problem of high-specific surface area nanometer rare earth oxide porous aerogel.In addition, this method is widely applicable, raw material is easy to get, with low cost, all has great importance for fields such as high-performance fluorescent material, metallurgical addition agent, catalyst, high-temperature superconductor, Solid State Laser, high temperature thermoelectricity and glass ceramics additives.
Description of drawings
The photo of Fig. 1 embodiment 1 sample.
The x x ray diffraction collection of illustrative plates of Fig. 2 embodiment 1 sample.
The FFIR figure of Fig. 3 embodiment 1 sample.
The electron scanning micrograph of Fig. 4 embodiment 1 sample.
The nitrogen adsorption desorption graph of pore diameter distribution of Fig. 5 embodiment 1 sample.
The photo of Fig. 6 embodiment 2 samples.
The x x ray diffraction collection of illustrative plates of Fig. 7 embodiment 2 samples.
The FFIR figure of Fig. 8 embodiment 2 samples.
The electron scanning micrograph of Fig. 9 embodiment 2 samples.
The nitrogen adsorption desorption graph of pore diameter distribution of Figure 10 embodiment 2 samples.
The specific embodiment
Below through implementing and accompanying drawing further specifies the present invention.(each raw material is marketable material, does not have the purity of special instruction and is chemical pure or analyzes pure grade)
Embodiment 1: the preparation of high-specific surface area low-density lanthana base aeroge
Ratio with lanthanum chloride, ethanol, deionized water, polyacrylic acid and expoxy propane is 6 mmol:50 ml:0.65 ml:0.78 ml:1.26 ml, under well-beaten situation, adds each reactant successively, obtains gel after leaving standstill.Gel carries out supercritical fluid drying after replacing three times through ethanol, finally can obtain the block lanthana base aerogel material that density is low to moderate about 50 mg/cc, and its photo in kind is as shown in Figure 1.
Shown in Figure 2, the x x ray diffraction spectrum of sample and 65-3185 standard card coincide, and the main component that this material is described is the cubic system lanthana of low-crystallinity.And shown in Figure 3, the FFIR of sample then shows, contains polyacrylic derivative in the sample, and the bridge-type complexing has taken place for lanthana and polyacrylic acid.Electron scanning micrograph among Fig. 4 then shows, this material has the loose structure of the mutual perforation that the network of nanometer scale forms.The nitrogen adsorption desorption graph of pore diameter distribution of Fig. 5 proves further that then this material also has the fine structure about 4 nm, and the specific area of sample is up to 229.1 m
2/ g.Integration test is the result show, this material is the lanthana base aeroge with multilevel hierarchy.
Embodiment 2: the preparation of high-specific surface area low-density yttria-base aeroge
Ratio with yttrium chloride, ethanol, deionized water, polyacrylic acid and expoxy propane is 6 mmol:60 ml:0.65 ml:0.78 ml:1.26 ml, under well-beaten situation, adds each reactant successively, obtains gel after leaving standstill.Gel carries out supercritical fluid drying after replacing three times through ethanol, finally can obtain the block yttria-base aerogel material that density is low to moderate about 60 mg/cc, and its photo in kind is as shown in Figure 6.
Shown in Figure 7, the x x ray diffraction spectrum of sample and 74-2350 standard card coincide, and the main component that this material is described is the monoclinic system aqua oxidation yttrium of low-crystallinity.And shown in Figure 8, the FFIR of sample then shows, contains polyacrylic derivative in the sample, and the bridge-type complexing has taken place for yittrium oxide and polyacrylic acid.Electron scanning micrograph among Fig. 9 then shows, this material has the loose structure of the mutual perforation that the network of nanometer scale forms.The nitrogen adsorption desorption graph of pore diameter distribution of Figure 10 then further the proof, this material also have micropore (<2 nm), mesoporous (2-50 nm) and macropore (>50 nm) multilevel hierarchy, and the specific area of sample is up to 229.6 m
2/ g.Integration test is the result show, this material is the yttria-base aeroge with multilevel hierarchy.
Embodiment3: the low cost of Ce/Nd composite rare-earth oxide aeroge sill preparation under the pure water solvent condition
Ratio with mixed chloride, deionized water and the expoxy propane of Ce and Nd (mol ratio 1:1) is 6 mmol:30 ml:1 ml (organic solvent and complexing agent are 0 ml); Under well-beaten situation, add each reactant successively, obtain gelatinous precipitate after leaving standstill.Deposition directly places the air dry of air normal pressure not have obvious reduction until quality, can obtain Ce/Nd composite rare-earth oxide aeroge based powders.
Embodiment4: the preparation of Pr/Sm/Eu ternary compound rare-earth oxide silica aerogel sill under the no complexing agent condition
Ratio with mixed chloride, acetonitrile, deionized water and the expoxy propane of Pr/Sm/Eu (mol ratio 0.05:0.05:1) is 6 mmol:10 ml:15 ml:2 ml (complexing agent is 0 ml); Under well-beaten situation, add each reactant successively, obtain gelatinous precipitate after leaving standstill.Deposition directly places the air dry of air normal pressure not have obvious reduction until quality, can obtain Pr/Sm/Eu ternary compound rare-earth oxide silica aerogel based powders.
EmbodimentThe preparation of 5:Dy/Gd/Er ternary compound rare-earth oxide silica aerogel sill
Ratio with mixed chloride, acetone, deionized water, acetylacetone,2,4-pentanedione and the epoxychloropropane of Dy/Gd/Er (mol ratio 0.05:0.1:1) is 6 mmol:20 ml:0.5 ml:2 ml:5 ml; Under well-beaten situation, add each reactant successively, obtain gelatinous precipitate after leaving standstill.Deposition can obtain Dy/Gd/Er ternary compound rare-earth oxide silica aerogel based powders after through 50 ℃ of heat de-airing dryings (vacuum drying).
EmbodimentThe preparation of 6:Tb/Ho/Er ternary compound rare-earth oxide silica aerogel sill
Ratio with mixed chloride, methyl alcohol, deionized water, acetate and the oxirane of Tb/Ho/Er (mol ratio 0.2:0.1:1) is 6 mmol:20 ml:20 ml:5 ml:10 ml; Under well-beaten situation, add each reactant successively, obtain gelatinous precipitate after leaving standstill.Carry out freeze drying after washing of deposition process and the solvent replacing, obtain Tb/Ho/Er ternary compound rare-earth oxide silica aerogel based powders at last.
EmbodimentThe preparation of 7:Tm/Yb/Lu/Y quaternary composite rare-earth oxide aeroge sill
Ratio with mixed chloride, ethanol, deionized water, polyacrylic acid and the expoxy propane of Tm/Yb/Lu/Y (mol ratio 0.05:0.05:0.05:1) is 6 mmol:20 ml:0.65 ml:0.78 ml:2 ml; Under well-beaten situation, add each reactant successively, obtain gel after leaving standstill.Gel carries out supercritical fluid drying after replacing three times through ethanol, finally can obtain block Tm/Yb/Lu/Y quaternary composite rare-earth oxide base aerogel material.
Above-described embodiment has been merely explanation technological thought of the present invention and characteristics; Its purpose is to make those of ordinary skill in the art can understand content of the present invention and implements according to this; The scope of this patent also not only is confined to above-mentioned specific embodiment; Be all equal variation or modifications of doing according to disclosed spirit, still be encompassed in protection scope of the present invention.
Claims (6)
1. the general preparation method of a high-specific surface area nanometer rare earth oxide porous aerogel material is characterized in that adopting inorganic dispersion sol-gal process, and concrete steps are following:
(1) the rare earth element chloride is dissolved in organic solvent and water mixed solution or directly soluble in water, is mixed with the rare earth element chloride solution;
(2) in the solution of step (1) gained, add complexing agent and epoxides successively, stir, obtain gel after leaving standstill; Wherein, the adding proportion of rare earth element chloride, organic solvent, water, complexing agent, epoxides is 6mmol:0 ~ 60ml:0.5 ~ 30ml:0-5ml:1-10ml;
(3) the aging at normal temperatures back of step (2) gained gel is dry, promptly obtain required rare earth oxide aerogel material.
2. preparation method according to claim 1 is characterized in that the rare earth element chloride described in the step (1) is lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium), any one or more mixture in ytterbium, lutetium or the yttrium chloride.
3. preparation method according to claim 1 is characterized in that the organic solvent described in step (1) and the step (2) is in methyl alcohol, ethanol, acetone or the acetonitrile any.
4. preparation method according to claim 1, it is characterized in that the complexing agent described in the step (2) be in acetate, acetylacetone,2,4-pentanedione or the polyacrylic acid any.
5. preparation method according to claim 1, it is characterized in that the epoxides described in the step (2) be in expoxy propane, oxirane or the epoxychloropropane any.
6. preparation method according to claim 1, it is characterized in that drying means described in the step (3) be in supercritical fluid drying, freeze drying, heat de-airing drying or the normal pressure air dry any.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104607116A (en) * | 2015-01-12 | 2015-05-13 | 朱秀榕 | Universal preparation method of high-specific surface area rare earth element-doped carbon gas gel |
| CN105536805A (en) * | 2015-12-10 | 2016-05-04 | 复旦大学 | Nanometer copper-cerium composite oxide catalyst, and preparation method and application thereof |
| CN105549065A (en) * | 2015-12-09 | 2016-05-04 | 中国船舶重工集团公司第七一九研究所 | Artificial radioactive aerosol source machine |
| CN110723778A (en) * | 2019-09-26 | 2020-01-24 | 浙江海洋大学 | Method for degrading polycyclic aromatic hydrocarbon in wastewater by acetone enhancement light |
| CN112058314A (en) * | 2020-08-31 | 2020-12-11 | 安徽壹石通材料科技股份有限公司 | Normal-pressure preparation method of rare earth oxide blended cerium oxide aerogel |
| CN112771205A (en) * | 2018-10-31 | 2021-05-07 | 日本钇股份有限公司 | Cold spray coating material |
| CN115448719A (en) * | 2022-10-11 | 2022-12-09 | 西安交通大学 | High-entropy block ceramic aerogel with high-temperature stability and preparation method and application thereof |
| CN115465878A (en) * | 2022-08-29 | 2022-12-13 | 山东大学 | Bulk nanocrystalline yttrium oxide aerogel and preparation method and application thereof |
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Cited By (14)
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| CN104607116A (en) * | 2015-01-12 | 2015-05-13 | 朱秀榕 | Universal preparation method of high-specific surface area rare earth element-doped carbon gas gel |
| CN105549065B (en) * | 2015-12-09 | 2018-12-18 | 中国船舶重工集团公司第七一九研究所 | A kind of artificial radioactive aerosol source machine |
| CN105549065A (en) * | 2015-12-09 | 2016-05-04 | 中国船舶重工集团公司第七一九研究所 | Artificial radioactive aerosol source machine |
| CN105536805B (en) * | 2015-12-10 | 2020-12-22 | 复旦大学 | Nano copper-cerium composite oxide catalyst and preparation method and application thereof |
| CN105536805A (en) * | 2015-12-10 | 2016-05-04 | 复旦大学 | Nanometer copper-cerium composite oxide catalyst, and preparation method and application thereof |
| CN112771205A (en) * | 2018-10-31 | 2021-05-07 | 日本钇股份有限公司 | Cold spray coating material |
| CN112771205B (en) * | 2018-10-31 | 2023-06-02 | 日本钇股份有限公司 | Material for cold spraying |
| TWI818105B (en) * | 2018-10-31 | 2023-10-11 | 日商日本釔股份有限公司 | Materials for cold spray |
| CN110723778A (en) * | 2019-09-26 | 2020-01-24 | 浙江海洋大学 | Method for degrading polycyclic aromatic hydrocarbon in wastewater by acetone enhancement light |
| CN112058314A (en) * | 2020-08-31 | 2020-12-11 | 安徽壹石通材料科技股份有限公司 | Normal-pressure preparation method of rare earth oxide blended cerium oxide aerogel |
| CN112058314B (en) * | 2020-08-31 | 2023-01-13 | 安徽壹石通材料科技股份有限公司 | Normal-pressure preparation method of rare earth oxide blended cerium oxide aerogel |
| CN115465878A (en) * | 2022-08-29 | 2022-12-13 | 山东大学 | Bulk nanocrystalline yttrium oxide aerogel and preparation method and application thereof |
| CN115465878B (en) * | 2022-08-29 | 2023-07-14 | 山东大学 | Bulk nanocrystalline yttrium oxide aerogel and preparation method and application thereof |
| CN115448719A (en) * | 2022-10-11 | 2022-12-09 | 西安交通大学 | High-entropy block ceramic aerogel with high-temperature stability and preparation method and application thereof |
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Application publication date: 20120926 |