CN101817544B - Method for preparing aluminum-cerium dual-component hydrosol - Google Patents
Method for preparing aluminum-cerium dual-component hydrosol Download PDFInfo
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- CN101817544B CN101817544B CN201010141234XA CN201010141234A CN101817544B CN 101817544 B CN101817544 B CN 101817544B CN 201010141234X A CN201010141234X A CN 201010141234XA CN 201010141234 A CN201010141234 A CN 201010141234A CN 101817544 B CN101817544 B CN 101817544B
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Abstract
The invention relates to a method for preparing dual-component hydrosol with a dispersed-phase aluminum component of boehmite nanometer crystal grains and a cerium component of cerianite nanometer crystal grains, and belongs to the field of inorganic nanometer materials. The method comprises the following steps of: adding alkali into mixed solution of Al3+ and Ce3+ salts to co-precipitate two kinds of metal ions; adding an oxidizing agent to oxidize Ce(OH)3 in the precipitate into overoxidation hydroxide of Ce4+; performing thermal decomposition on the overoxidation hydroxide of Ce4+ in the precipitate to form Ce(OH)4 (cerium hydroxide (IV)); and adding acid to peptize the precipitate to prepare boehmite-cerianite sol. The clear boehmite-cerianite dual-component hydrosol can be prepared by the method, and the dispersed phase of the hydrosol consists of nanometer crystal grains; and the crystal grains are not agglomerated and are uniform in size, and the size is generally 3 nanometers.
Description
Technical field
The al compsn that the present invention relates to a kind of aluminium, cerium dual-component hydrosol, particularly a kind of disperse phase is that γ-AlOOH (boehmite) is nanocrystalline, the cerium component is CeO
2(with CeO
2Unique crystalline phase side cerium stone occur mutually) preparation method of nanocrystalline dual-component hydrosol; Be that nm boehmite-square cerium stone dual-component hydrosol (is the easy meter of narration; When mentioning this boehmite-square cerium stone dual-component hydrosol, it is abbreviated as " aluminium cerium colloidal sol " below) wet chemical preparation method.The invention belongs to field of inorganic nano material.
Background technology
Having aspect the colloidal sol technology of preparing of certain correlationship with the present invention, bibliographical information focuses mostly in single boehmite sol preparation.Because coarse-grained side's cerium stone deposition is difficult to peptization, makes to be difficult for preparing stable CeO
2The water-sol.The prior art of this respect appears among the patent ZL 99114762.6, and it relates to a kind of CeO
2The compound method of the water-sol, it is an initiator with the aqueous solution of the mixed chlorinated rare earth that contains cerium (III), through the steps such as oxyhydroxide of deposition-oxidation-selective dissolution non-Ce rare earth, acquisition CeO
2Nano-sized hydrosol, this colloidal sol can long-term stability be deposited.In addition, Dong Xiangting etc. is with ammonia precipitation process Ce (NO
3)
3, with nitric acid peptization deposition, obtain CeO then
2Can more stably there be 48h [.CeO such as Dong Xiangting in nano-sized hydrosol, the light yellow transparent water-sol of gained
2The preparation of nano-sized hydrosol. Rare Metals Materials and engineering, 2002,31 (3): 229～231].Rare report aluminium, preparation method, the especially aluminium of cerium dual-component hydrosol, the preparation method of cerium dual-component nano-sized hydrosol.
The present invention has arranged Al
3+, Ce
3+The quick co-precipitation-cerium in the throw out (III) is oxidized to cerium (IV)-peptization by γ-AlOOH and Ce (OH)
4The sedimentary technology that (cerous hydroxide (IV)) constitutes is prepared aluminium cerium colloidal sol, constitutes the aluminium of the disperse phase of this water-sol, the crystalloid compound that the cerium particulate is several nanoscales.The researchist in present technique field knows, under acid solution effect with concentration, and Ce (OH)
4And the solubleness of γ-AlOOH is well below Ce (OH)
3Solubleness.The researchist in present technique field also knows, the oxyhydroxide Ce (OH) of cerium (IV)
4Pairing complete dewatered product is CeO
2, still, Ce (OH)
4The side's of having cerium stone (CeO
2Unique crystalline phase) crystalline structure, Ce (OH)
4Same CeO
2Between difference only be that the former is moisture, that is: Ce (OH)
4Can be counted as a kind of aqueous CeO
2, be expressed as two hydration cerium dioxide (CeO
22H
2O).And Ce (OH)
4Partly dehydrating changes CeO at a lower temperature
2MH
2O (m＜2) for example realizes under the hydrothermal condition of T≤100 ℃.That is to say hydration cerium dioxide (CeO
2NH
2O, n≤2) with crystalloid CeO
2Crystalline structure consistent.The hot analytical results of hydration cerium dioxide matches with this understanding: raise with temperature, the hydration cerium dioxide dewaters gradually, when dehydration reaches complete, changes CeO into
2, phase transformation does not appear in this process.Oxyhydroxide Ce (OH) with cerium (IV)
4Above-mentioned character distinctly be the oxyhydroxide Ce (OH) of cerium (III)
3The product of dehydration is crystalloid Ce
2O
3, crystalloid Ce
2O
3Crystalline structure be different from Ce (OH)
3Crystalline structure; The product of γ-AlOOH dehydration is crystalloid Al
2O
3, crystalloid Al
2O
3Crystalline structure be different from the crystalline structure of γ-AlOOH; Here, crystalloid oxyhydroxide adheres to two crystalloid structures separately with the corresponding crystalloid oxide compound that is formed by their dehydrations.The present invention utilizes the oxyhydroxide Ce (OH) of cerium (IV) just
4And the characteristic of the oxyhydroxide γ-AlOOH of aluminium, provide a kind of from Al
3+, Ce
3+The mixing solutions of salt sets out, and synthesizes the technology of stable aluminium cerium dual-component nanocrystalline colloidal sol.
Summary of the invention
The al compsn that the object of the present invention is to provide a kind of preparation aluminium cerium colloidal sol, particularly a kind of disperse phase is the method for the dual-component hydrosol that boehmite is nanocrystalline, the cerium component side of being cerium stone is nanocrystalline.
According to the foregoing invention purpose, preparation method of the present invention, the preparation method of aluminium cerium colloidal sol realizes that through following technical scheme this scheme has been characterised in that following process step:
(1) according to n
Al: n
Ce=x: 1 molar ratio is got solubility Al
3+Salt and Ce
3+The salt batching makes aluminium cerium dual-component solution; Under violent stirring, in this solution, add alkali lye fast, make its moment that Al take place
3+, Ce
3+Co-precipitation, generate by γ-AlOOH and Ce (OH)
3The white powder jelly shape thing that constitutes;
(2) under violent stirring, in the jelly shape thing that step (2) is obtained, add oxygenant, oxidation Ce (OH)
3For Ce (OOH) (OH)
3(Ce
4+The hydrogen peroxide oxidation thing), make white jelly shape thing change the maroon suspension liquid into, viscosity obviously reduces;
(3) the HV suspension liquid that obtained of heated and boiled step (3) takes off for faint yellow suspension liquid gradually, and viscosity reduces greatly, and the solid particulate in this faint yellow suspension liquid is by γ-AlOOH and Ce (OH)
4Constitute;
(4) under violent stirring; Slow dripping dilute acid reduces the pH value of suspension liquid gradually in the LV suspension liquid that step (3) is obtained, and accompanies with it; The turbidity of suspension liquid also reduces gradually; As clear as crystal until changing into, this limpid liquid is the dispersed system of nm boehmite-square cerium stone, i.e. aluminium cerium colloidal sol.
Al in the above-mentioned steps (1)
3+Salt is a kind of in aluminum chloride, aluminum nitrate, the Burow Solution.
Ce in the above-mentioned steps (1)
3+Salt is a kind of in cerous chlorate, the cerous nitrate.
Alkali lye in the above-mentioned steps (1) is ammoniacal liquor.
Oxygenant in the above-mentioned steps (2) is a ydrogen peroxide 50.
Diluted acid in the above-mentioned steps (4) is a kind of in hydrochloric acid, the nitric acid.
The concentration of the diluted acid in the above-mentioned steps (4) is 1.00mol/l～3.00mol/l.
The pH value of the aluminium cerium colloidal sol that above-mentioned steps (4) is obtained is 1.2～2.0.
Preparing method of the present invention is through adding fast alkali lye in aluminium, cerium mixing solutions, pH value moment of solution is elevated to Al
3+And Ce
3+More than the ionic deposition pH value, make Al
3+And Ce
3+Ion is transformed into γ-AlOOH and Ce (OH) rapidly
3White powder jelly shape coprecipitate.Know, concentration be the aluminum ion of 1mol/l to begin sedimentary pH value be 3.3, precipitate completely that the pH value is 5.2, to begin sedimentary pH value be 7.6 and concentration is cerium (III) ion of 1mol/l.If change the adding mode of alkali lye, in this two-pack solution, slowly add alkali lye, the pH value of solution is raise gradually, in the process of this pH value gradual change, at first sedimentary will be Al
3+Ion, after the aluminum ion deposition is complete, Ce
3+Ion just begins deposition, because two types of sedimentary priorities form, the differentiation deposition of two hydroxide will occur and grows up.In a simultaneous test; When other condition is identical; Can't realize complete peptization through adding acid in the later stage by the formed deposit seeds of slow adding alkali lye, even the pH value of the faint yellow suspension liquid that step (3) is obtained is lowered to below 1.0, suspension liquid still can not be dissolved clearly.Above-mentioned condition test explanation, the differentiation deposition trend that suppresses two components is vital to the limpid colloidal sol of the final acquisition of the present invention.
Preparing method of the present invention is through add ydrogen peroxide 50, the Ce (OH) in the oxidation precipitation fast in above-mentioned white powder jelly shape thing
3Particulate be cerium (IV) hydrogen peroxide oxidation thing Ce (OOH) (OH)
3, the pH value of solution is dropped to～7.
The maroon HV suspension liquid that preparation method of the present invention is obtained through heated and boiled step (2), the peroxide bridge of the hydrogen peroxide oxidation thing of decomposition cerium (IV) makes it change the oxyhydroxide Ce (OH) of cerium (IV) into
4
Preparing method of the present invention is contained γ-AlOOH and Ce (OH) through what obtain to step (3)
4Slow dripping dilute acid in the sedimentary suspension liquid makes to constitute sedimentary coacervate particle generation peptization.Peptization is that a kind of temporal aggregate that makes is that the colloidal particle of coacervate is dispersed in the process that forms colloidal solution (being colloidal sol) in the liquid phase again.Construction features as the coacervate of peptization object of the present invention are γ-AlOOH and Ce (OH)
4The distribution that in the coacervate particle, adjoins each other of two kinds of nanoparticles.In the peptization course, a kind of nanoparticle all will help disengaging, the dispersion of another kind of particulate, thereby help finally forming the two-pack Nano sol from disengaging, the dispersion of such coacervate particle surface.Peptization course of the present invention relates to the effect of two aspects simultaneously: on the one hand being that the part boehmite is dissolved and destroy coacervate agglomeration of particles structure, is disengaging, the dispersion of nanoparticle from the coacervate surface on the other hand.In the peptization pH value scope that the present invention arranged, intravital Ce (OH) reunites
4Particulate can stable existence, and the part boehmite can be dissolved, and this part boehmite should be the relative chump of structural integrity, and this solvency action will help the coacervate particle and disintegrate; Add-on with acid solution increases; The nanoparticle that is positioned at coacervate surface is charged and be tending towards at the outside stable surface charge layer that forms of particulate because of the absorption positively charged ion; Under suitably mechanical force (as stirring) acted on, these charged corpuscles can be separated from from the coacervate surface, are dispersed in the liquid phase.This effect down collaborative aspect two, net result is that the coacervate particle disintegrates fully, forms with Ce (OH)
4For main body, the γ-AlOOH of disperse phase is accessory aluminium cerium colloidal sol.
Substantive distinguishing features of the present invention is, has γ-AlOOH and Ce (OH) as the coacervate particle of peptization object
4Two kinds of structural attitudes that nanoparticle adjoins each other and distributes, this structural attitude is to make Al through quick adding alkali lye
3+And Ce
3+Ion rapidly, synchronously forms precipitation of hydroxide, then in time with the Ce in the coprecipitate (OH)
3Particulate changes Ce (OH) into
4And realize.Since with the acid solution of concentration to Ce (OH)
4Dissolving power be far smaller than it to Ce (OH)
3Dissolving power, therefore, with Ce (OH)
3Particulate changes Ce (OH) into
4, be that preparation method of the present invention is able to one of key condition that obtains by aluminium cerium colloidal sol.If there is not this transformation, adding acid downward modulation γ-AlOOH-Ce (OH)
3During the pH value of suspension liquid, Ce (OH)
3Particulate is very easily dissolved, and the peptization product that is generated in such cases will be to be scattered in CeCl
3-AlCl
3Boehmite sol in the solution, and can't form aluminium cerium colloidal sol.
The present invention has following advantage and unusual effect:
One, the prepared aluminium cerium colloidal sol of the present invention is nm boehmite (γ-AlOOH)-square cerium stone (CeO
2) colloidal sol, that is: aluminium, the cerium oxide particles of formation colloidal sol disperse phase are nanocrystalline.This aluminium cerium colloidal sol is transparent, stable, can place for a long time and turbidization, gelation etc. not take place.The purposes of the nanocrystalline aluminium cerium colloidal sol that present method is prepared has two.The one, this colloidal sol is used for dip-coating is carried out on the surface of different shape carrier (for example ball, pipe, plate, rod etc.), generate crystalline boehmite-square cerium stone surface film at carrier surface; Through selecting the number of times of repetition dip-coating, just can control the crystalloid coating thickness of carrier surface.The 2nd, directly coagulation goes out nm boehmite-square cerium stone flour body from this colloidal sol.Because the dispersed system that this aluminium cerium colloidal sol is boehmite and square cerium stone nanoparticle uses the rete of this colloidal sol preparation and powder to be crystalline state without calcining; If gained rete or powder are calcined, raise with calcining temperature, with the boehmite dehydration that makes one of composition, change the serial isomer of aluminum oxide into, promptly generate from γ-Al
2O
3(low temperature product) is to α-Al
2O
3The series of phase transitions product of (high-temperature product), and square cerium stone no phase transformation and variation of valence in calcination process.Know CeO
2The composite oxides of base are the basal component of handling the catalytic conversion agent of vehicle exhaust, to CeO
2Interior doped gamma-Al
2O
3The time, can optimize CeO
2The oxygen surge capability.Simultaneously, γ-Al
2O
3-CeO
2Mixture still is the good an acidic catalyst and the combustioncatalysts of aromatic compound.From the prepared crystalloid aluminium cerium colloidal sol of present method, be easy to obtain nanometer γ-AlOOH-CeO
2And nanometer Al
2O
3-CeO
2The compact film of mixture or fine powder are because their high-specific surface area and high reactivity make the function of mixture be able to optimize.
Two, the preparation technology of the present invention's employing can suppress the differentiation deposition trend of aluminium, cerium component in co-precipitation step, and makes γ-AlOOH and the Ce (OH) as the peptization object
4Individual fine nature remains to before the peptization always, thereby has guaranteed that last precipitation-peptization is smooth.In concrete process step is arranged, when realizing Al
3+, Ce
3+Quick co-precipitation after, in time in system, add oxygenant, with oxidation Ce (OH)
3For Ce (OOH) (OH)
3, and making the viscosity of system that obvious reduction arranged, the pH value is dropped rapidly to nearly neutrality.This disposal is handled with heated and boiled subsequently and is combined, and transforms effectively with γ-AlOOH and coexists as the Ce (OH) in the deposit seeds
3Be Ce (OH)
4This processing arrangement makes as the γ-AlOOH and the Ce (OH) of peptization object
4Particulate is able to keep fine nature, and has guaranteed that the compound of cerium can keep stable in peptization course.In peptization course, realize the peptization dispersion of being partly dissolved of boehmite and hydroxide particulate through the adding of diluted acid, thereby destroy γ-AlOOH and Ce (OH) in the coacervate particle
4The adjacency structure of two kinds of nanoparticles makes the Ce (OH) that is difficult to peptization usually
4From deposit seeds, dissociate smoothly,, with peptization dispersive nm boehmite together, form the two-pack nano-sized hydrosol with nanocrystalline individual dispersion suspension.This preparation technology has overcome Ce (OH)
4Be difficult to by the problem of peptization, and need not to be used in combination auxiliary peptization means such as reflux, ultra-sonic dispersion.
Three, colloidal sol preparation technology of the present invention is simple and easy to do.From Al
3+And Ce
3+The ionic co-precipitation is to coacervate particulate peptization, and four steps are accomplished without any letup in same reaction vessel, has realized that a cooking-pot type is synthetic.
Embodiment
Below in conjunction with embodiment preparation method of the present invention is further described, following embodiment will help to understand the present invention, but not limit content of the present invention.
Embodiment 1
A kind of method for preparing nano aluminum cerium colloidal sol of the present invention, its process step is following:
(1) uses CeCl
37H
2O makes the solution 600ml that concentration is 0.20mol/l, and according to Al: Ce=0.25: 1 molar ratio is to wherein adding AlCl
36H
2O gets colourless transparent solution after the dissolving.Under violent stirring, impouring 60ml strong aqua in solution makes solution moment change white powder jelly shape thing into.
(2) add the 30ml ydrogen peroxide 50 rapidly, make white jelly shape thing become maroon HV suspension liquid.
(3) suspension liquid that heated and boiled obtained takes off for faint yellow up to suspension liquid, and its viscosity reduces greatly.
(4) stir down, the Hydrogen chloride that slowly drips concentration while hot and be 2.00mol/l carries out peptization to slurries, makes it change the yellow-green colour vitreosol gradually into, and its pH value is 1.55.
Confirm by chemical analysis; In the obtained colloidal sol of present embodiment; Dissolved colloidal state aluminium (being the boehmite particle) accounts for 15.3% of total aluminium mole number; Dissolved colloidal state cerium (side's of being cerium stone particle) accounts for 97.7% of total cerium mole number, and the disperse phase that the obtained colloidal sol of present embodiment is described is to be main ingredient with square cerium stone particle, and the boehmite particle is an accessory constituent.The high-resolution-ration transmission electric-lens of the obtained colloidal sol of present embodiment (HRTEM) pictorial display, each intercrystalline does not have reunion, and the size of crystal grain is even, is roughly 3nm, and the positively charged ion of nanocrystal is arranged regular substantially, can tell lattice fringe; Some nanocrystalline individualities are carried out the fourier transformation image, and diffraction spot is carried out exponentiate, and then the diffraction pattern of the side's of determining that it is cerium stone monocrystalline.
The shelf stability of the prepared aluminium cerium of present method colloidal sol is good, and one glass of colloidal sol sample sealing and standing that is made by embodiment 1 is deposited and reached more than 1 year, and is still as clear as crystal, do not have any deposition and separates out, and also do not form gel.
Embodiment 2
A kind of method for preparing nano aluminum cerium colloidal sol of the present invention, its raw material and process step are similar to embodiment 1, but in step (1) according to Al: Ce=0.11: 1 molar ratio is to CeCl
3Add AlCl in the solution
36H
2O, step (4) uses concentration as the Hydrogen chloride of 1.00mol/l slurries to be carried out peptization, makes it change the yellow-green colour vitreosol gradually into.
The pH value of the obtained colloidal sol of present embodiment is 1.24, and dissolved colloidal state aluminium accounts for 29.8% of total aluminium mole number, and the dissolved colloidal state cerium accounts for 98.2% of total cerium mole number.
Embodiment 3
A kind of method for preparing nano aluminum cerium colloidal sol of the present invention, its raw material and process step are similar to embodiment 1, but in step (1) according to Al: Ce=0.43: 1 molar ratio is to CeCl
3Add AlCl in the solution
36H
2O, step (4) uses concentration as the Hydrogen chloride of 3.00mol/l slurries to be carried out peptization, makes it change the yellow-green colour vitreosol gradually into.
The pH value of the obtained colloidal sol of present embodiment is 1.96, and dissolved colloidal state aluminium accounts for 20.2% of total aluminium mole number, and the dissolved colloidal state cerium accounts for 97.4% of total cerium mole number.
Embodiment 4
A kind of method for preparing nano aluminum cerium colloidal sol of the present invention, its process step is similar to embodiment 1, but employed raw material is different from embodiment 1, and this place is with Ce (NO
3)
36H
2O and Al (NO
3)
39H
2O is as starting material, and according to Al: Ce=0.25: 1 molar ratio batching, step (4) use concentration as rare nitric acid of 2.00mol/l slurries to be carried out peptization, make it change the yellow-green colour vitreosol gradually into.
The pH value of the obtained colloidal sol of present embodiment is 1.33, and dissolved colloidal state aluminium accounts for 17.5% of total aluminium mole number, and the dissolved colloidal state cerium accounts for 96.8% of total cerium mole number.
Claims (8)
1. the preparation method of boehmite-square cerium stone dual-component hydrosol is characterized in that having following process step:
(1) according to n
Al: n
Ce=x: 1 molar ratio batching, in the formula, composition parameter x is 0.11～0.43, preparation solubility Al
3+Salt and Ce
3+The aqueous solution of salt adds alkali with the impouring mode in this solution under stirring fast, obtains Al
3+, Ce
3+Coprecipitate;
(2) under agitation, add oxygenant in time fast, obtain to contain boehmite and the sedimentary suspension liquid of hydrogen peroxide oxidation cerium (IV);
(3) under agitation, heated and boiled step (2) suspension liquid that obtains obtains containing the sedimentary suspension liquid of boehmite and cerous hydroxide (IV);
(4) under agitation, slowly add acid,, promptly obtain boehmite-square cerium stone dual-component hydrosol up to the complete peptization of throw out.
2. the preparation method of boehmite according to claim 1-square cerium stone water-sol is characterized in that the solubility Al of said step (1)
3+Salt is aluminum chloride, aluminum nitrate or Burow Solution, solubility Ce
3+Salt is cerous chlorate or cerous nitrate.
3. the preparation method of boehmite according to claim 1-square cerium stone water-sol, the alkali that it is characterized in that said step (1) is ammoniacal liquor.
4. the preparation method of boehmite according to claim 1-square cerium stone water-sol, the oxygenant that it is characterized in that said step (2) is a ydrogen peroxide 50.
5. the preparation method of boehmite according to claim 1-square cerium stone water-sol, the acid that it is characterized in that said step (4) is hydrochloric acid or nitric acid.
6. the preparation method of boehmite according to claim 1-square cerium stone water-sol, the concentration that it is characterized in that the acid of said step (4) is 1.00mol/l～3.00mol/l.
7. the preparation method of side's cerium stone-boehmite sol according to claim 1 is characterized in that the pH value that makes the complete peptization of throw out of said step (4) is 1.2～2.0.
8. the preparation method of boehmite according to claim 1-square cerium stone water-sol is characterized in that the disperse phase of said boehmite-square cerium stone water-sol is made up of boehmite and square cerium stone nano crystal.
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| CN108311156A (en) * | 2018-02-01 | 2018-07-24 | 广州市新稀冶金化工有限公司 | Based on nano rare-earth hydrosol without alum denitrating catalyst and preparation method thereof |
| CN109761259B (en) * | 2019-03-27 | 2021-04-02 | 淄博加华新材料有限公司 | Preparation method of cerium glue with high gelling property |
| CN111792660A (en) * | 2020-07-15 | 2020-10-20 | 东北大学 | Method for producing boehmite micro-nano powder by using aluminum chloride |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1269327A (en) * | 1999-04-01 | 2000-10-11 | 张其春 | Technological process of preparing pure cerium hydroxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1269327A (en) * | 1999-04-01 | 2000-10-11 | 张其春 | Technological process of preparing pure cerium hydroxide |
Non-Patent Citations (4)
| Title |
|---|
| S. PICKERING et al..Preparation and properties of alumina-ceria nano-nano composites.《JOURNAL OF MATERIALS SCIENCE》.1999,第34卷2.1节. * |
| 刘连利等.二氧化铈/氧化铝纳米复合粉体的制备及抗紫外线性能研究.《无机盐工业》.2010,第42卷(第3期),第1.2节、第2.1节. * |
| 宋晓岚等.共沉淀法合成CeO2/γ-Al2O3复合纳米晶的研究.《稀土》.2004,第25卷(第6期),1.1节. * |
| 董相廷等.CeO2纳米水溶胶的制备.《稀有金属材料与工程》.2002,第31卷(第3期),1.1节. * |
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