CN100460061C - Method for preparing nano-Ce-Magnesium coumpoud oxide - Google Patents
Method for preparing nano-Ce-Magnesium coumpoud oxide Download PDFInfo
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- CN100460061C CN100460061C CNB2007100391749A CN200710039174A CN100460061C CN 100460061 C CN100460061 C CN 100460061C CN B2007100391749 A CNB2007100391749 A CN B2007100391749A CN 200710039174 A CN200710039174 A CN 200710039174A CN 100460061 C CN100460061 C CN 100460061C
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Abstract
The present invention relates to two methods for preparing nanometre Ce-Mg composite oxide, which belongs to the superfine Ce-Mg composite oxide powder preparation field. Sol gel method has the reaction material of cerium nitrate hexahydrate and basic magnesium carbonate, and has a complexing agent of malic acid, wherein the cerous nitrate and the basic magnesium carbonate are dissolved in water respectively and then are mixed with each other, then malic acid is added therein before agitating at room temperature, and then ammonia liquor is dropped therein to adjust the pH value, so as to obtain nanometre Ce-Mg composite oxide after evaporating solvent, drying and calcining. The self-propagating combustion method has reaction substrate of cerium nitrate hexahydrate and magnesium nitrate, and has a complexing agent of malic acid, wherein the malic acid is dissolved in water, then cerous nitrate and magnesium nitrate are added therein synchronously before agitating at room temperature, and then ammonia liquor is dropped therein to adjust the pH value, so as to obtain nanometre Ce-Mg composite oxide after evaporating solvent, drying and calcining. The two methods can all obtain Ce-Mg composite oxide powder having a small particle diameter, a uniform dispersion and a large specific surface.
Description
Technical field
The present invention relates to two kinds of methods that prepare nano-Ce-Magnesium coumpoud oxide, belong to ultra-fine Ce-Magnesium coumpoud oxide powder preparing technical field.
Background technology
Nano-Ce-Magnesium coumpoud oxide is a kind of novel multifunctional nano material with perovskite structure, has a wide range of applications.Nano-Ce-Magnesium coumpoud oxide because of have than single rare earth oxide ceria preferably resistance to elevated temperatures be applied even more extensively in vehicle exhaust and handle and other catalytic fields.In the Industrial Catalysis process, also can be used as the carrier or the co-catalyst of catalyst.(400nm～700nm) has high permeability and (200nm～400nm) has strong absorbability to ultraviolet light because nano-Ce-Magnesium coumpoud oxide is to visible light, therefore, can be used for the anti-aging of rubber, the antiultraviolet material, can also be mixed and made into advanced composite material (ACM) with fluorescent material adds in the fluorescent tube, sponge the mankind are harmful to and to the influential ultraviolet light of lamp tube service life, and do not reduce the luminous efficiency of fluorescent material, thereby can improve the service life and the safety in utilization of fluorescent lamp.
The main preparation methods of nano composite oxide has: the precipitation method, sol-gal process, solid reaction process, microemulsion method etc.But the precipitation method are more to the influence factor of product, make condition restive, and need high-temperature calcination, and equipment is required height, power consumption greatly; The solid phase method reaction is inhomogeneous, causes the gained sample particle not of uniform size, disperses inhomogeneous; Microemulsion method is also very unripe on production technology, still can not be applied to suitability for industrialized production on a large scale, in addition, this method cost of material height, often organic solvent will be used in the preparation process or Organic Ingredients pollutes environment, and the gained presoma needs high-temperature process.Sol-gal process uses metal alkoxide as raw material usually in the prior art, causes cost higher and have certain toxicity, and environment protecting is relatively poor; From the method that spreads is raw material with the citric acid usually, is used to prepare oxide, is used to prepare nano-Ce-Magnesium coumpoud oxide at present and does not appear in the newspapers as yet.Because there is the production cost height to some extent in above-mentioned these methods, complex manufacturing, severe reaction conditions, shortcomings such as product price height and environmental pollution are restricted its application in suitability for industrialized production.The used sol-gal process of this experiment can overcome the shortcomings and deficiencies of additive method, has reaction evenly, and is low for equipment requirements, advantages such as easy operating.
Summary of the invention
The purpose of this invention is to provide two kinds of methods that prepare nano-Ce-Magnesium coumpoud oxide that reaction is even, with low cost, i.e. collosol and gel method and self-propagating combustions.
By sol-gal process provided by the invention and self-propagating combustion, it is little all can to obtain particle diameter, is uniformly dispersed the Ce-Mg composite oxide powder that specific surface is big.In addition, can obtain the composite oxides of different cerium magnesium proportionings by the control material rate, and can be by control reaction condition, the size of regulating the nano material particle diameter.And the present invention synthesizes two kinds of new Ce-Magnesium coumpoud oxides, i.e. Ce first
0.4Mg
0.6O
1.4And Ce
0.6Mg
0.4O
1.6
For realizing purpose of the present invention, adopt following technical scheme:
One, adopts the Prepared by Sol Gel Method nano-Ce-Magnesium coumpoud oxide
With six water cerous nitrates and basic magnesium carbonate is reaction raw materials, and malic acid is a complexing agent.Cerous nitrate and basic magnesium carbonate back soluble in water are respectively mixed, add malic acid then, stir under the room temperature, dropping ammonia is regulated the pH value, through evaporating solvent, obtains nano-Ce-Magnesium coumpoud oxide after drying and the calcining.This scheme is characterised in that, is respectively cerium source and magnesium source with six water cerous nitrates and basic magnesium carbonate, is complexing agent with the malic acid, is n (Ce in molar ratio with cerous nitrate and basic magnesium carbonate
3+): n (Mg
2+)=1:9～9:1 mixes back soluble in water, press malic acid again and be (0.5～2) with total metal ion mol ratio: 1 adds malic acid, stirred 1～4 hour under the room temperature of dissolving back, in above-mentioned mixed liquor, add ammoniacal liquor, the pH value of solution is adjusted between 5.0～9.0,50 ℃～80 ℃ following evaporating solvents get wet gel, got loose porous xerogel in 3～10 hours 50 ℃～120 ℃ following vacuum drying then, with xerogel be put in the Muffle furnace in 500 ℃～600 ℃ down calcining 2～4 hours Powdered target product, i.e. nano-Ce-Magnesium coumpoud oxide.
The advantage of this technical scheme:
(1) raw materials used being easy to get is cheap, and preparation cost is low, and operating process is simple, and be low for equipment requirements, do not have the loss of raw material in the preparation process, and it is few to form accessory substance, has reduced the pollution to environment, the productive rate height;
(2) initiative is a complexing agent with the malic acid, forms the good complex compound of dispersive property with metal ion in solution and colloidal sol, has guaranteed the ultra-fine grain diameter of gained target product;
(3) by control proportion of raw materials, the pH value of solution, the calcining heat and the calcination time of presoma, can make the nano-Ce-Magnesium coumpoud oxide of different cerium magnesium proportionings, also can control the particle diameter and the pattern of target product.
Two, adopt self-propagating combustion to prepare nano-Ce-Magnesium coumpoud oxide
With six water cerous nitrates and magnesium nitrate is reaction substrate, and malic acid is a complexing agent.Malic acid is soluble in water, add cerous nitrate and magnesium nitrate after the dissolving simultaneously, stir under the room temperature, dropping ammonia is regulated the pH value, through evaporating solvent, drying and heating, obtains nano-Ce-Magnesium coumpoud oxide behind self-propagating combustion.This scheme is characterised in that, be respectively cerium source and magnesium source with six water cerous nitrates and magnesium nitrate, with the malic acid is complexing agent, press malic acid and be (0.5～2): a certain amount of malic acid of 1 weighing with total metal ion mol ratio, with malic acid soluble in water after, be n (Ce with cerous nitrate and magnesium nitrate by certain molar ratio
3+): n (Mg
2+)=1:9～9:1 adds in the malic acid solution simultaneously, stir 1～4h under the room temperature of dissolving back, in above-mentioned mixed liquor, add the pH value of ammoniacal liquor regulator solution between 1.0～6.0,50 ℃～80 ℃ following evaporating solvents obtain wet gel, get loose porous xerogel at 50 ℃～90 ℃ vacuum drying 3～10h then.Placing on the heating plate xerogel directly, heating makes its self-propagating combustion get Powdered target product, i.e. nano-Ce-Magnesium coumpoud oxide.
The advantage of this technical scheme:
(1) raw materials used being easy to get is cheap, and preparation cost is low, and operating process is simple, and be low for equipment requirements, do not have the loss of raw material in the preparation process, and it is few to form accessory substance, has reduced the pollution to environment, the productive rate height; Realize suitability for industrialized production easily;
(2) initiative is a complexing agent with the malic acid, malic acid is brought into play two important effects in reaction: 1. malic acid forms the good complex compound of dispersive property with metal ion in solution and colloidal sol, guaranteed the ultra-fine grain diameter of gained target product, 2. malic acid has played reducing agent, cause self-propagating combustion with nitrate ion, the heat that this redox reaction produces has satisfied the needs that continue reaction, and the reaction time can be shortened, owing to do not need high-temperature process, energy savings significantly, simultaneously because the reaction time weak point, temperature is low, helps the refinement of particle, can also reduce interparticle reunion degree;
(3) by the proportioning of control reactant and the pH value of solution, can prepare the particle diameter nano-Ce-Magnesium coumpoud oxide different, also can make the nano-Ce-Magnesium coumpoud oxide of different cerium magnesium proportionings with pattern.
Description of drawings
Fig. 1 is the TEM figure of the nano Ce MgO3 that obtains after 600 ℃ of calcinings
Fig. 2 is the XRD figure of different cerium magnesium proportionings: (a) CeMgO
3(b) Ce
0.4Mg
0.6O
1.4(c) Ce
0.6Mg
0.4O
1.6(d) Ce
0.1Mg
0.9O
1.1(e) Ce
0.9Mg
0.1O
1.9
Fig. 3 is the ultraviolet-visible spectrum of different cerium magnesium proportionings: (a) CeMgO
3(b) Ce
0.4Mg
0.6O
1.4(c) Ce
0.6Mg
0.4O
1.6(d) Ce
0.1Mg
0.9O
1.1(e) Ce
0.9Mg
0.1O
1.9
The specific embodiment
Sol-gal process:
Embodiment 1:
With six water cerous nitrates and five scale formula magnesium carbonate is cerium source and magnesium source, malic acid is a complexing agent, get 0.4857g five scale formula magnesium carbonate and 2.1713g six water cerous nitrates and be dissolved in back mixing in the 15ml water respectively, add malic acid 0.6707g again, the mol ratio of cerium ion and magnesium ion is 1:1, malic acid is 0.5:1 with the mol ratio of total metal ion, after the dissolving, stir 2h under the room temperature, dropping ammonia is regulated pH=5.00,50 ℃ of constant temperature are put into vacuum drying chamber in 60 ℃ of dry 3h again until forming gel then, the xerogel of bulk multi-hole.Be placed in the Muffle furnace at 500 ℃, calcining 3h, pale yellow powder shape product, nano Ce MgO3.
Embodiment 2:
With six water cerous nitrates and five scale formula magnesium carbonate is cerium source and magnesium source, malic acid is a complexing agent, get 0.8747g five scale formula magnesium carbonate and 0.4346g six water cerous nitrates and be dissolved in back mixing in the 15ml water respectively, add malic acid 1.3413g again, the mol ratio of cerium ion and magnesium ion is 1:9, malic acid is 1:1 with the mol ratio of total metal ion, after the dissolving, stir 3h under the room temperature, dropping ammonia is regulated pH=6.00,60 ℃ of constant temperature are until forming gel then, put into 80 ℃ of vacuum drying chambers dry 5h down again, the xerogel of bulk multi-hole.Be placed on and calcine 2h in the Muffle furnace under 600 ℃, get pale yellow powder shape product, nano Ce 0.1Mg0.9O1.1.
Embodiment 3:
With six water cerous nitrates and five scale formula magnesium carbonate is cerium source and magnesium source, malic acid is a complexing agent, get 0.0972g five scale formula magnesium carbonate and 3.9082g six water cerous nitrates and be dissolved in back mixing in the 15ml water respectively, add malic acid 2.6817g again, the mol ratio of cerium ion and magnesium ion is 9:1, malic acid is 2:1 with the mol ratio of total metal ion, after the dissolving, stir 4h under the room temperature, dropping ammonia is regulated pH=7.00,70 ℃ of constant temperature are put into vacuum drying chamber in 100 ℃ of dry 7h again until forming gel then, the xerogel of bulk multi-hole.Be placed in the Muffle furnace at 500 ℃, calcining 3h, pale yellow powder shape product, nano Ce 0.9Mg0.1O1.9.
Embodiment 4:
With six water cerous nitrates and five scale formula magnesium carbonate is cerium source and magnesium source, malic acid is a complexing agent, get 0.3886g five scale formula magnesium carbonate and 2.6053g six water cerous nitrates and be dissolved in back mixing in the 15ml water respectively, add malic acid 2.0114g again, the mol ratio of cerium ion and magnesium ion is 6:4, malic acid is 1.5:1 with the mol ratio of total metal ion, after the dissolving, stir 4h under the room temperature, dropping ammonia is regulated pH=8.00,70 ℃ of constant temperature are put into vacuum drying chamber in 110 ℃ of dry 8h again until forming gel then, the xerogel of bulk multi-hole.Be placed in the Muffle furnace at 500 ℃, calcining 4h, pale yellow powder shape product, nano Ce 0.6Mg0.4O1.6.
Embodiment 5:
With six water cerous nitrates and five scale formula magnesium carbonate is cerium source and magnesium source, malic acid is a complexing agent, get 0.5831g five scale formula magnesium carbonate and 1.7369g six water cerous nitrates and be dissolved in back mixing in the 15ml water respectively, add malic acid 2.0115g again, the mol ratio of cerium ion and magnesium ion is 4:6, malic acid is 1.5:1 with the mol ratio of total metal ion, after the dissolving, stir 4h under the room temperature, dropping ammonia is regulated pH=9.00,80 ℃ of constant temperature are put into vacuum drying chamber in 120 ℃ of dry 7h again until forming gel then, the xerogel of bulk multi-hole.Be placed in the Muffle furnace at 500 ℃, calcining 3h, pale yellow powder shape product, nano Ce 0.4Mg0.6O1.4.
Self-propagating combustion:
Embodiment 6:
With six water cerous nitrates and magnesium nitrate hexahydrate is cerium source and magnesium source, malic acid is a complexing agent, getting the 0.6705g malic acid is dissolved in the 30ml distilled water, add 2.1716g six water cerous nitrates and 1.2820g magnesium nitrate hexahydrate after the dissolving simultaneously, the mol ratio of cerium ion and magnesium ion is 1:1, the mol ratio of malic acid and metal ion is 0.5:1, treat that it all stirs 2h under the room temperature of dissolving back, dropping ammonia is regulated pH=1.00,50 ℃ of following constant temperature are put into 70 ℃ of following dry 3h of vacuum drying chamber again until forming gel, get the xerogel of bulk multi-hole, place on the heating plate directly heating to make it that self-propagating combustion take place xerogel, obtain pale yellow powder shape nano Ce MgO3.
Embodiment 7:
With six water cerous nitrates and magnesium nitrate hexahydrate is cerium source and magnesium source, malic acid is a complexing agent, getting the 1.3411g malic acid is dissolved in the 30ml distilled water, add 0.4345g six water cerous nitrates and 2.3081g magnesium nitrate hexahydrate after the dissolving simultaneously, the mol ratio of cerium ion and magnesium ion is 1:9, the mol ratio of malic acid and metal ion is 1:1, treat that it all stirs 3h under the room temperature of dissolving back, dropping ammonia is regulated pH=2.00,60 ℃ of following constant temperature are until forming gel, put into 80 ℃ of following dry 5h of vacuum drying chamber again, get the xerogel of bulk multi-hole.Place on the heating plate directly heating to make it that self-propagating combustion take place xerogel, obtain pale yellow powder shape nano Ce 0.1Mg0.9O31.1.
Embodiment 8:
With six water cerous nitrates and magnesium nitrate hexahydrate is cerium source and magnesium source, malic acid is a complexing agent, getting the 2.0114g malic acid is dissolved in the 30ml distilled water, add 3.9086g six water cerous nitrates and 0.2567g magnesium nitrate hexahydrate after the dissolving simultaneously, the mol ratio of cerium ion and magnesium ion is 9:1, the mol ratio of malic acid and metal ion is 1.5:1, treat that it all stirs 4h under the room temperature of dissolving back, dropping ammonia is regulated pH=3.00,70 ℃ of following constant temperature are until forming gel, put into 90 ℃ of following dry 7h of vacuum drying chamber again, get the xerogel of bulk multi-hole, place on the heating plate directly heating to make it that self-propagating combustion take place xerogel, obtain pale yellow powder shape nano Ce 0.9Mg0.1O1.9.
Embodiment 9:
With six water cerous nitrates and magnesium nitrate hexahydrate is cerium source and magnesium source, malic acid is a complexing agent, getting the 2.6821g malic acid is dissolved in the 30ml distilled water, add 2.6055g six water cerous nitrates and 1.0257g magnesium nitrate hexahydrate after the dissolving simultaneously, the mol ratio of cerium ion and magnesium ion is 6:4, the mol ratio of malic acid and metal ion is 2:1, treat that it all stirs 4h under the room temperature of dissolving back, dropping ammonia is regulated pH=4.00,80 ℃ of following constant temperature are put into 80 ℃ of following dry 8h of vacuum drying chamber again until forming gel, get the xerogel of bulk multi-hole, place on the heating plate directly heating to make it that self-propagating combustion take place xerogel, obtain pale yellow powder shape nano Ce 0.6Mg0.4O1.6.
Embodiment 10:
With six water cerous nitrates and magnesium nitrate hexahydrate is cerium source and magnesium source, malic acid is a complexing agent, getting the 1.3410g malic acid is dissolved in the 30ml distilled water, add 1.7371g six water cerous nitrates and 1.5385g magnesium nitrate hexahydrate after the dissolving simultaneously, the mol ratio of cerium ion and magnesium ion is 4:6, the mol ratio of malic acid and metal ion is 1:1, treat that it all stirs 4h under the room temperature of dissolving back, dropping ammonia is regulated pH=6.00,80 ℃ of following constant temperature are put into 80 ℃ of following dry 10h of vacuum drying chamber again until forming gel, get the xerogel of bulk multi-hole, place on the heating plate directly heating to make it that self-propagating combustion take place xerogel, obtain pale yellow powder shape nano Ce
0.4Mg
0.6O
31.4
Claims (2)
1. the preparation method of a nano-Ce-Magnesium coumpoud oxide adopts sol-gal process, it is characterized in that being respectively cerium source and magnesium source with six water cerous nitrates and basic magnesium carbonate, and with the malic acid complexing agent, be n (Ce in molar ratio with six water cerous nitrates and basic magnesium carbonate
3+): n (Mg
2+)=1:9～9:1 mixes back soluble in water, press malic acid again and be (0.5～2) with total metal ion mol ratio: 1 adds malic acid, stirred 1～4 hour under the room temperature of dissolving back, in the gained mixed liquor, add ammoniacal liquor, the pH value of solution is adjusted between 5.0～9.0,50 ℃～80 ℃ following evaporating solvents get wet gel, got loose porous xerogel in 3～10 hours 50 ℃～120 ℃ following vacuum drying then, xerogel is calcined down in 500 ℃～600 ℃ got Powdered nano-Ce-Magnesium coumpoud oxide in 2～4 hours.
2. the preparation method of a nano-Ce-Magnesium coumpoud oxide, adopt self-propagating combustion, it is characterized in that being respectively cerium source and magnesium source with six water cerous nitrates and magnesium nitrate, with the malic acid is complexing agent, is (0.5～2) in malic acid with total metal ion mol ratio: 1 ratio, with malic acid soluble in water after, be n (Ce with six water cerous nitrates and magnesium nitrate by certain molar ratio
3+): n (Mg
2+)=1:9～9:1 adds in the malic acid solution simultaneously, stirred 1～4 hour under the room temperature of dissolving back, in the gained mixed liquor, add the pH value of ammoniacal liquor regulator solution between 1.0～6.0,50 ℃～80 ℃ following evaporating solvents obtain wet gel, got loose porous xerogel in 3～10 hours 50 ℃～90 ℃ vacuum drying then, xerogel is placed directly to heat on the heating plate make its self-propagating combustion get Powdered nano-Ce-Magnesium coumpoud oxide.
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| CN109111230B (en) * | 2018-10-31 | 2020-12-29 | 航天特种材料及工艺技术研究所 | Yttrium oxide-magnesium oxide nano composite powder and preparation method thereof |
| CN110876386B (en) * | 2019-11-20 | 2022-01-14 | 厦门稀土材料研究所 | Rare earth oxide and nano-silver synergistic antibacterial agent and preparation method thereof |
| CN115385377B (en) * | 2022-08-25 | 2023-10-24 | 湖南汇帮环保科技有限公司 | Preparation method of copper chromite for laser engraving chemical plating auxiliary |
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| CN1887718A (en) * | 2006-08-01 | 2007-01-03 | 华东师范大学 | Combustion process of preparing nanometer CeO2 |
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| CN1789132A (en) * | 2005-12-07 | 2006-06-21 | 华东师范大学 | Method for preparing ultrafine nano-magnesia |
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