CN103641146A - Preparation method of uniformly dispersed fusiform cerium carbonate particles - Google Patents
Preparation method of uniformly dispersed fusiform cerium carbonate particles Download PDFInfo
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- CN103641146A CN103641146A CN201310640020.0A CN201310640020A CN103641146A CN 103641146 A CN103641146 A CN 103641146A CN 201310640020 A CN201310640020 A CN 201310640020A CN 103641146 A CN103641146 A CN 103641146A
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Abstract
The invention discloses a preparation method of uniformly dispersed fusiform cerium carbonate particles. The method is characterized by comprising the steps: in a liquid phase precipitation system simulating a biomineralization environment, by utilizing a non-ionic surfactant alkylphenol polyoxyethylene ether as a template agent and soluble cerium salt as a raw material, adding a precipitating agent containing carbonate and carrying out aging, filtering and drying, thus preparing the uniformly dispersed fusiform cerium carbonate particles, wherein a long axis and short axis of a fusiform surface are respectively 5-8mu m and 1.5-3.5mu m and the thickness of the fusiform surface is 2-5mu m. The preparation method has the advantages that an ethyoxyl long chain of alkylphenol polyoxyethylene ether is utilized; through lattice matching and stereochemical structure complementation, the non-ionic surfactant has the functions of spatial orientation and spatial constraint to control the nucleation process and crystal growth, so that the size, morphology and structure of the cerium carbonate crystal are controlled and adjusted. The raw materials are low in price and the method and equipment are simple, are convenient to operate and easily achieve industrial production.
Description
Technical field
The invention belongs to the preparation field of powder body material, relate to a kind of method of utilizing the synthetic fusiformis cerous carbonate particle of nonionogenic tenside template to regulate.Specifically, in the liquid-phase precipitation system of simulation biomineralization environment, utilize nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7 as template, solubility cerium salt, as raw material, adds the precipitation agent containing carbonate, through ageing, filtration, oven dry, prepare homodisperse fusiformis shape cerous carbonate particle, this fusiformis face length axle is 5～8 μ m, and minor axis is 1.5～3.5 μ m, and thickness is 2～5 μ m.
Background technology
Baotou rare earth aboundresources, and the feature of Baotou rare earth resource is to occupy an leading position with light rare earths, and wherein cerium content accounts for 50%, therefore develops cerium resources advantage particularly important.
Cerium oxide uniqueness store oxygen function and the quick oxygen of high temperature room diffusibility, be widely used in the fields such as electronic ceramics, glass polishing, luminescent material, vehicle exhaust processing, catalysis, in modern high technology field, have huge development potentiality.
The inorganic materials that synthetic form, size and structure are subject to artificial adjustment is an important research direction of modern material science.
By the method for biomineralization be incorporated into material synthetic in, under the regulation and control of all kinds of organic additives and template, be expected to realize the effective adjusting to inorganics morphology, preparation has the material of unique microstructure characteristic and performance.After roasting, crystal morphology has heredity, and the morphology control of presoma is good, and the pattern of product cerium oxide is just controlled.
At present, the cerium oxide of various patterns and performance all studies have reported that, as cerium oxide pore size material, self-assembled material, functional materials, nanotube, nanometer rod etc.Although it is a lot of to prepare the method for cerium oxide, be not also applicable at present the method for large-scale commercial production.
The research of the cerium oxide that pattern is controlled mostly adopts hydrothermal method, and utilizes nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7 as template, and synthetic fusiformis cerous carbonate have not been reported.
Summary of the invention
The technical issues that need to address of the present invention are just to overcome the defect of prior art, a kind of preparation method of homodisperse fusiformis cerous carbonate particle is provided, it utilizes nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7 ethoxylated long chain to be adsorbed on cerous carbonate plane of crystal, by lattice match and stereochemical structure complementation, there is the effect of spatial positioning and space constraint, control cerous carbonate nucleation process and crystal growth etc., make the size of presoma cerous carbonate crystal, pattern, structure is controlled and adjusting all, obtain particle size even, the fusiformis shape cerous carbonate particle of pattern rule.
For addressing the above problem, the present invention adopts following technical scheme:
The invention provides a kind of preparation method of homodisperse fusiformis cerous carbonate particle, described method is in the liquid-phase precipitation system of simulation biomineralization environment, utilize nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7 as template, solubility cerium salt, as raw material, adds the precipitation agent containing carbonate, through ageing, filtration, oven dry, prepare homodisperse fusiformis shape cerous carbonate particle, this fusiformis face length axle is 5～8 μ m, and minor axis is 1.5～3.5 μ m, and thickness is 2～5 μ m.
Particularly, described method comprises the steps:
(1) cerium solution that compound concentration is 1.55mol/L, adjust pH is 5～12, gets this solution 1.5～16.5ml in beaker, adds water to 133ml; Take nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7 liquid, add water 100ml and dissolve; Nonionic surfactant solution is stirred and adds cerium solution to evenly, obtain mixed solution, make [Ce
3+] be 0.01～0.11mol/L, agent induced by alkyl hydroxybenzene Soxylat A 25-7 concentration is 0.3～1.2g/L;
(2) take precipitation agent, making precipitation agent and the quality of cerium oxide is 1～2 than ratio, is dissolved in water, and making the concentration of precipitation agent is 0.01～0.10mol/L, is uniformly mixed;
(3) precipitant solution of being prepared by step (2) adds in mixed solution prepared by step (1), and feed time is 0.1～2h, and precipitant solution adds rear continuation and stirs 0.5h, and ageing 0.1～48h filters, and washing, after oven dry, obtains fusiformis cerous carbonate particle.
In the present invention, described cerium salt is water-soluble cerium salt, and described water-soluble cerium salt is cerous nitrate, Cerium II Chloride, cerous acetate or cerous sulfate.
In the present invention, described precipitation agent is the soluble carbonate salt containing carbonate; The described soluble carbonate salt containing carbonate is volatile salt, bicarbonate of ammonia or sodium carbonate.
In the present invention, described nonionogenic tenside is induced by alkyl hydroxybenzene Soxylat A 25-7, and described induced by alkyl hydroxybenzene Soxylat A 25-7 comprises polyoxyethylene nonylphenol ether (NPEO), polyoxyethylene octylphenol ether (OPEO), alkylpolyoxyethylene (DPEO) or Dinonylphenol Polyoxyethylene Ether (DNPEO).
In the present invention, deionized water washing 3 times for the filter cake after filtration, alcohol wash 2 times, dries 2h, obtains homodisperse fusiformis cerous carbonate particle for 60 ℃.
The present invention selects nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7 as template, the liquid-phase precipitation system of simulation biomineralization environment, prepares homodisperse fusiformis shape cerous carbonate particle, and this fusiformis face length axle is 5～8 μ m, minor axis is 1.5～3.5 μ m, and thickness is 2～5 μ m.
Advantage of the present invention:
The present invention simulates the liquid-phase precipitation system of biomineralization environment and prepares fusiformis cerous carbonate particle, and whole reaction process is at room temperature carried out, and reaction conditions is gentle, and method is simple, is easy to control.
The present invention is the pattern as template regulation and control cerous carbonate with nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7 first, and method is simple, be easy to control, and prepares fusiformis cerous carbonate particle.This nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7 ethoxylated long chain is adsorbed on cerous carbonate plane of crystal, by lattice match and stereochemical structure complementation, there is the effect of spatial positioning and space constraint, be controlled to nuclear process and crystal growth etc., make size, pattern, all controlled and adjustings of structure of cerous carbonate crystal.
Accompanying drawing explanation
Fig. 1 [Ce
3+] be 0.05mol/L, [NPEO] is the SEM picture of the synthetic cerous carbonate of 0g/L.
Fig. 2 [Ce
3+] be 0.05mol/L, [NPEO] is the SEM picture of the synthetic cerous carbonate of 0.6g/L.
Fig. 3 [Ce
3+] be 0.05mol/L, [OPEO] is the SEM picture of the synthetic cerous carbonate of 0.9g/L.
Fig. 4 [Ce
3+] be 0.05mol/L, [DPEO] is the SEM picture of the synthetic cerous carbonate of 1.2g/L.
Fig. 5 [Ce
3+] be 0.05mol/L, [DNPEO] is the SEM picture of the synthetic cerous carbonate of 1.5g/L.
Fig. 6 [Ce
3+] be 0.11mol/L, [NPEO] is 0.6g/L, pH is the SEM picture of 5 synthetic cerous carbonates.
Fig. 7 [Ce
3+] be 0.11mol/L, [NPEO] is 0.6g/L, pH is the SEM picture of 7 synthetic cerous carbonates.
Fig. 8 [Ce
3+] be 0.11mol/L, [NPEO] is 0.6g/L, pH is the SEM picture of 9 synthetic cerous carbonates.
Fig. 9 [Ce
3+] be 0.11mol/L, [NPEO] is 0.6g/L, pH is the SEM picture of 11 synthetic cerous carbonates.
Embodiment
(NH used in the specific embodiment of the invention
4)
2cO
3, NH
4hCO
3for Tianjin reagent three factories, induced by alkyl hydroxybenzene Soxylat A 25-7 is East China, Tianjin chemical reagent work, and ethanol is analytical pure product.
embodiment 1
Do not add induced by alkyl hydroxybenzene Soxylat A 25-7 carbonate synthesis cerium particle, as a comparison experiment:
(1) cerous nitrate solution that compound concentration is 1.55mol/L, adjust pH is 5, gets this solution 7.5ml in 1000ml beaker, adds water to 233ml, makes [Ce
3+] be 0.05mol/L;
(2) take precipitation agent volatile salt 3g, add water 625mL and dissolve, be uniformly mixed;
(3) with peristaltic pump, precipitant solution is joined in cerium solution, feed time is 1h, and 0.5h is stirred in the rear continuation of having fed in raw material, ageing 4h, and suction filtration, dries, and obtains the cerous carbonate particle of random sheet, as shown in Figure 1.
embodiment 2
(1) cerous nitrate solution that compound concentration is 1.55mol/L, adjust pH is 5, gets this solution 7.5ml in 1000ml beaker, adds water to 133ml; Take nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7 liquid, add water 100ml and dissolve; Add cerium solution to evenly nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7 solution stirring, make [Ce
3+] be 0.05mol/L, [NPEO] is 0.6g/L;
(2) take precipitation agent volatile salt 3g, add water 625mL and dissolve, be uniformly mixed;
(3) with peristaltic pump, precipitant solution is joined in the mixing solutions of cerous nitrate and nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7, feed time is 1h, and 0.5h is stirred in the rear continuation of having fed in raw material, ageing 4h, suction filtration, dries, obtain fusiformis cerous carbonate particle, as shown in Figure 2.
embodiment 3
(1) cerous nitrate solution that compound concentration is 1.55mol/L, adjust pH is 5, gets this solution 7.5ml in 1000ml beaker, adds water to 133ml; Take nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7 liquid, add water 100ml and dissolve; Add cerium solution to evenly nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7 solution stirring, make [Ce
3+] be 0.05mol/L, [OPEO] is 0.9g/L, or [DPEO] be 1.2g/L, or [DNPEO] is 1.5g/L;
(2) take precipitation agent volatile salt 3g, add water 625mL and dissolve, be uniformly mixed;
(3) with peristaltic pump, precipitant solution is joined in the mixing solutions of cerous nitrate and nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7, feed time is 1h, and 0.5h is stirred in the rear continuation of having fed in raw material, ageing 4h, suction filtration, dries, obtain fusiformis cerous carbonate particle, as shown in Fig. 3, Fig. 4 and Fig. 5.
embodiment 4
(1) cerous nitrate solution that compound concentration is 1.55mol/L, adjust pH is 5～12, gets this solution 16.5ml in 1000ml beaker, adds water to 133ml; Take nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7 liquid, add water 100ml and dissolve; Add cerium solution to evenly nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7 solution stirring, make [Ce
3+] be 0.11mol/L, [NPEO] is 0.6g/L;
(2) take precipitation agent volatile salt 3g, add water 625mL and dissolve, be uniformly mixed;
(3) with peristaltic pump, precipitant solution is joined in the mixing solutions of cerous nitrate and cationic polyelectrolyte, feed time is 1h, and 0.5h is stirred in the rear continuation of having fed in raw material, ageing 4h, suction filtration, dries, obtain fusiformis cerous carbonate particle, as shown in Fig. 6, Fig. 7, Fig. 8 and Fig. 9.
Finally it should be noted that: obviously, above-described embodiment is only for example of the present invention is clearly described, and the not restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without also giving all embodiments.And the apparent variation of being amplified out thus or change are still among protection scope of the present invention.
Claims (6)
1. the preparation method of a homodisperse fusiformis cerous carbonate particle, it is characterized in that: described method is in the liquid-phase precipitation system at simulation biomineralization environment, utilize nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7 as template, solubility cerium salt, as raw material, adds the precipitation agent containing carbonate, through ageing, filtration, oven dry, prepare homodisperse fusiformis shape cerous carbonate particle, this fusiformis face length axle is 5～8 μ m, and minor axis is 1.5～3.5 μ m, and thickness is 2～5 μ m.
2. the preparation method of homodisperse fusiformis cerous carbonate particle as claimed in claim 1, is characterized in that, described method comprises the steps:
(1) cerium solution that compound concentration is 1.55mol/L, adjust pH is 5～12, gets this solution 1.5～16.5ml in beaker, adds water to 133ml; Take nonionogenic tenside induced by alkyl hydroxybenzene Soxylat A 25-7 liquid, add water 100ml and dissolve; Nonionic surfactant solution is stirred and adds cerium solution to evenly, obtain mixed solution, make [Ce
3+] be 0.01～0.11mol/L, agent induced by alkyl hydroxybenzene Soxylat A 25-7 concentration is 0.3～1.2g/L;
(2) take precipitation agent, making precipitation agent and the quality of cerium oxide is 1～2 than ratio, is dissolved in water, and making the concentration of precipitation agent is 0.01～0.10mol/L, is uniformly mixed;
(3) precipitant solution of being prepared by step (2) adds in mixed solution prepared by step (1), and feed time is 0.1～2h, and precipitant solution adds rear continuation and stirs 0.5h, and ageing 0.1～48h filters, and washing, after oven dry, obtains fusiformis cerous carbonate particle.
3. the preparation method of homodisperse fusiformis cerous carbonate particle as claimed in claim 2, is characterized in that, described cerium salt is water-soluble cerium salt, and described water-soluble cerium salt is cerous nitrate, Cerium II Chloride, cerous acetate or cerous sulfate.
4. the preparation method of homodisperse fusiformis cerous carbonate particle as claimed in claim 3, is characterized in that: described precipitation agent is the soluble carbonate salt containing carbonate; The described soluble carbonate salt containing carbonate is volatile salt, bicarbonate of ammonia or sodium carbonate.
5. the preparation method of homodisperse fusiformis cerous carbonate particle as claimed in claim 4, it is characterized in that: described nonionogenic tenside is induced by alkyl hydroxybenzene Soxylat A 25-7, described induced by alkyl hydroxybenzene Soxylat A 25-7 comprises polyoxyethylene nonylphenol ether (NPEO), polyoxyethylene octylphenol ether (OPEO), alkylpolyoxyethylene (DPEO) or Dinonylphenol Polyoxyethylene Ether (DNPEO).
6. the preparation method of homodisperse fusiformis cerous carbonate particle as claimed in claim 5, is characterized in that: deionized water washing 3 times for the filter cake after filtration, alcohol wash 2 times, dries 2h, obtain homodisperse fusiformis cerous carbonate particle for 60 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107098374A (en) * | 2017-05-25 | 2017-08-29 | 内蒙古科技大学 | Dispersed bulk morphologies carbonic acid cerium crystal and preparation method thereof |
| CN113120942A (en) * | 2019-12-30 | 2021-07-16 | 安集微电子科技（上海）股份有限公司 | Synthesis method of spindle-shaped cerium carbonate and cerium oxide thereof |
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| CN1426963A (en) * | 2001-12-17 | 2003-07-02 | 暨南大学 | Manufacturing method of nano cerium oxide powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098374A (en) * | 2017-05-25 | 2017-08-29 | 内蒙古科技大学 | Dispersed bulk morphologies carbonic acid cerium crystal and preparation method thereof |
| CN113120942A (en) * | 2019-12-30 | 2021-07-16 | 安集微电子科技（上海）股份有限公司 | Synthesis method of spindle-shaped cerium carbonate and cerium oxide thereof |
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