CN109761258A - Amphipathic rod-like nano cerium oxide and amphipathic rodlike CeO2/Ce3+The preparation method of reactive nanoparticles - Google Patents
Amphipathic rod-like nano cerium oxide and amphipathic rodlike CeO2/Ce3+The preparation method of reactive nanoparticles Download PDFInfo
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Abstract
The invention discloses amphipathic rod-like nano cerium oxide and amphipathic rodlike CeO2/Ce3+The preparation method of reactive nanoparticles, wherein the preparation method of amphipathic rod-like nano cerium oxide includes preparing guiding agent aqueous solution and cerous salt aqueous solution；The guiding agent aqueous solution is mixed and the cerous salt aqueous solution obtains suspension；The still aging suspension obtains sediment；Washing, it is dry, roast the sediment and obtain the amphipathic rod-like nano cerium oxide；Amphipathic rodlike CeO2/Ce3+The preparation method of reactive nanoparticles, including the amphipathic rod-like nano cerium oxide is put into the second cerous salt aqueous solution and is stirred, the second sediment is obtained by filtration；Dry second sediment obtains the amphipathic rodlike CeO2/Ce3+Reactive nanoparticles；Solve the problems, such as that existing rod-like nano cerium oxide is difficult to prepare, polarity causes by force dispersion effect difference and activity not high.
Description
Technical field
The present invention relates to nano-cerium oxides and preparation method thereof.
Background technique
Rare earth element is a kind of permanent magnet, applies valence with high in rechargeable battery, catalyst and corrosion-inhibiting coating field
Value.In the derivative of Ce elements, cerium oxide is most commonly seen, especially nano-cerium oxide, due to catching with stronger cation
Ability, outstanding storage put oxygen performance and its strong absorbability to ultraviolet light are caught, in purifying vehicle exhaust, photochemical catalyst, machinery
The fields such as polishing, ultraviolet radiation absorption, fuel-cell electrolyte possess excellent properties and wide application prospect.Therefore, people
It is more and more to the research of nano-cerium oxide.With gradually going deep into for research, the preparation method of nano-cerium oxide is further more
Sample, common preparation method have hydro-thermal method, sol-gal process, microemulsion method and thermal decomposition method etc..But these methods are not only
Process is complicated, preparation step is cumbersome, will cause environmental pollution toward contact, therefore, it is difficult to carry out industry's enlarging production.
On the one hand, the pattern for the nano-cerium oxide prepared using these methods be also it is far from each other, such as rodlike, sheet,
Linear, spherical, flower-shaped, cube, octahedron etc..Many has preferential sudden and violent the study found that in many patterns mentioned above
Dew (100), the cerium oxide nano-rod of (110) crystal face or nanometer sheet can show more excellent storage put oxygen performance, catalysis is lived
Property and anti-corrosion effect.Researcher has had developed the preparation method of the nano-cerium oxide of many sheets, still, has reported in document
To method in, the preparation of rod-like nano cerium oxide, which rarely has, to be referred to.
On the other hand, the chemical property of pure zirconia cerium is stablized, and cannot be actively engaged in chemical reaction, this greatly limits
Its application in the fields such as catalysis and anti-corrosion.So needing to activate by certain means, its use scope of further expansion.
Finally, the wettability of material is very crucial on performance influence.Cerium oxide surface is hydrophilic and oleophobic property under normal circumstances
Very strong polarity is presented in matter, therefore is difficult in organic media evenly dispersed, is unfavorable for the performance of performance.And Normal practice one
As it is modified using surfactant, to improve disperse properties, but effect is undesirable.In addition, cerium oxide has very strong water imbibition
Limit its catalyze and synthesize, in terms of application, inside absorption water and can greatly reduce its usability in conjunction with water
It can, it is impossible to obtain long-acting high performance corrosion-inhibiting coating.
Summary of the invention
In view of this, the present invention provides a kind of amphipathic rod-like nano cerium oxide and amphipathic rodlike CeO2/Ce3+Activity is received
The preparation method of rice grain, solves that existing rod-like nano cerium oxide is difficult to prepare, polarity causes by force dispersion effect difference and activity not
High problem.
In a first aspect, a kind of preparation method of amphipathic rod-like nano cerium oxide, comprising:
Prepare guiding agent aqueous solution and cerous salt aqueous solution；
The guiding agent aqueous solution is mixed and the cerous salt aqueous solution obtains suspension；
The still aging suspension obtains sediment；
Washing, it is dry, roast the sediment and obtain the amphipathic rod-like nano cerium oxide.
Preferably, the guiding agent is citric acid or citrate.
Preferably, the concentration of the guiding agent aqueous solution is 0.03 ~ 4 mol/L.
Preferably, the cerous salt is one of cerous nitrate, cerous sulfate or cerium chloride.
Preferably, the concentration of the cerous salt aqueous solution is 0.04 ~ 5mol/L.
Preferably, the molar ratio of the guiding agent and the cerous salt is 1:5 ~ 5:1.
Preferably, the mixing guiding agent aqueous solution and the cerous salt aqueous solution, be at 0 ~ 50 DEG C and
Under the conditions of being stirred continuously, in Xiang Suoshu guiding agent aqueous solution, the cerous salt aqueous solution is added dropwise according to the speed of 0.5 ~ 3d/s,
Continue 0 ~ 10 h of stirring after being added dropwise.
Preferably, the time of the ageing be 6 ~ for 24 hours.
Preferably, the washing, using distilled water；The temperature of the drying is 60 ~ 100 DEG C, the time is 2 ~ 8h；The roasting
The temperature of burning is 400 ~ 550 DEG C, the time is 2 ~ 12h.
Preferably, the guiding agent aqueous solution, preparation method are as follows:
0.005 ~ 0.1mol guiding agent is taken in container and adds water to 15 ~ 25mL；
Stirring and dissolving obtains the guiding agent aqueous solution after ultrasonic disperse 5-10 min.
Preferably, the cerous salt aqueous solution, preparation method are as follows:
0.005 ~ 0.1mol cerous salt particle is taken in container and adds water to 5 ~ 15mL；
Stirring and dissolving obtains the cerous salt aqueous solution after ultrasonic disperse 5-10 min.
Second aspect provides a kind of amphipathic rodlike CeO2/Ce3+The preparation method of reactive nanoparticles, comprising:
The amphipathic rod-like nano cerium oxide is put into the second cerous salt aqueous solution and is stirred, the second precipitating is obtained by filtration
Object；
Dry second sediment obtains the amphipathic rodlike CeO2/Ce3+Reactive nanoparticles.
Preferably, the mixing time is 2-10h；The filtering, using being filtered under diminished pressure mode.
Preferably, the concentration of the second cerous salt aqueous solution is 0.08 ~ 3mol/L.
The invention has the following beneficial effects:
(1) preparation method of the present invention does not need hydro-thermal process, without using organic solvent, only at a lower temperature may be used yet
Directly obtain amphiphilic rodlike CeO2/Ce3+Reactive nanoparticles, and preparation process is simple, low energy consumption, pollution-free, is easy
It realizes technology production, solves the problems, such as that existing rod-like nano cerium oxide is difficult to prepare；
(2) due to the incomplete decomposing of citrate ion in roasting process, so that the rodlike CeO of active nano2Surface is attached with
A small amount of C element, therefore show hydrophilic, oleophylic amphipathic；
(3) by Ce3+Cerium oxide nano-rod in solution after ultrasound has higher reactivity.
Detailed description of the invention
By the description below with reference to attached drawing to the embodiment of the present invention, the above and other purposes of the present invention, feature and
Advantage is apparent, in the accompanying drawings:
Diagram 1 is the 1 amphipathic rodlike CeO of gained of embodiment2/Ce3+The XRD diagram of reactive nanoparticles proves that product is in figure
CeO2(comparison JCPDS card No. 898436).
Diagram 2 is the 1 amphipathic rodlike CeO of gained of embodiment2/Ce3+SEM the and EDS analysis chart of reactive nanoparticles, in figure
Prove resulting CeO2For rod-like nano particle, and surface is attached with a small amount of C element (presence of surface C element makes rodlike CeO2It receives
Rice grain has amphipathic).
Diagram 3 is the 1 amphipathic rodlike CeO of gained of embodiment2/Ce3+The XPS of reactive nanoparticles schemes (Ce 3d), demonstrate,proves in figure
Bright resulting amphipathic rod-like nano CeO2Contain Ce in surface3+(Ce3+Presence make CeO2With higher activity).
Diagram 4 is ceria nanoparticles (water suction oleophobic) and the 1 amphipathic rodlike CeO of gained of embodiment on the market2/Ce3 +Reactive nanoparticles prove resulting rodlike CeO in water phase and ultrasonic disperse effect contrast figure in oily phase, figure2/Ce3+Activity
Nano particle has amphipathic.
It is filler, with the oxidation of amphipathic rod-like nano that diagram 5, which is with ceria nanoparticles (water suction oleophobic) on the market,
Cerium is for filler and with amphipathic rodlike CeO2/Ce3+Reactive nanoparticles are dimethicone-epoxy coating of filler in 3.5% salt
Nyquist after water impregnates 60 days schemes comparison, which proves to contain amphipathic rodlike CeO after salt water impregnates 60 days2/Ce3+It is living
The corrosion resistance of the coating of property nano particle is more more prominent than other two coatings.It is proved in figure resulting amphipathic rodlike
CeO2/Ce3+The reactive nanoparticles activity with higher for inhibiting corrosion.
Specific embodiment
Below based on embodiment, present invention is described, but it is worth noting that, the present invention is not limited to these realities
Apply example.It is detailed to describe some specific detail sections below in datail description of the invention.However, for not detailed
The present invention can also be understood completely in the part described to the greatest extent, those skilled in the art.
Embodiment 1
One, prepared by product
It weighs 7g citric acid to be added in 20mL deionized water, is stirred well to and is completely dissolved, continue to stir under the conditions of 50 DEG C
12min.It weighs six nitric hydrate cerium of 5g and is added in 10mL deionized water and stir to being completely dissolved labeled as No. 1, then weigh 3g
It is number that six nitric hydrate ceriums, which are dissolved in label in 10mL deionized water,.Using acid buret by No. 1 solution according to the speed of 3d/s
Degree is added drop-wise to dropwise just in the citric acid solution of cooling and stirring, continues to be stirred to react 10min after being added dropwise.Then it precipitates molten
Liquid is aged 8h under the conditions of 50 DEG C, is filtered under diminished pressure, and adopts and dries 3h after being washed with deionized under the conditions of 70 DEG C, is placed in Muffle furnace
In roast 3h at 450 DEG C after obtain amphipathic rod-like nano cerium oxide.
Amphipathic rod-like nano cerium oxide is put into No. 2 solution, 10h is stirred by ultrasonic, obtains 2 institute of attached drawing after filtering, drying
The amphipathic rodlike CeO shown2/Ce3+Reactive nanoparticles.
Two, properties of product are tested
By amphipathic rodlike CeO2/Ce3+Reactive nanoparticles and common nano-cerium oxide divide after stirring in dimethicone
It is not added in epoxy coating, carries out EIS test after impregnating 60 days using 3.5% salt water, as a result as shown in figure 5, containing commonly receives
The capacitor arc of rice cerium oxide has been significantly less than the capacitor arc of the coating containing amphipathic rod-like nano cerium oxide.
It can be seen that from the said goods the performance test results due to amphipathic rodlike CeO2/Ce3+Reactive nanoparticles absorb
Part dimethicone, enhances itself barrier property to corrosive media, in addition, Ce3+It is gradually aoxidized in the coating
For CeO2Process provide the effect of cathodic protection for substrate, so amphipathic rodlike CeO2/Ce3+Reactive nanoparticles can be with
The service performance of nano-cerium oxide is improved, long-acting high performance corrosion-inhibiting coating is obtained, to preferably be applied to coating and catalysis
Equal fields, expand the use scope of nano-cerium oxide.
Embodiment 2
It weighs 15g citric acid to be added in 20mL deionized water, is stirred well to and is completely dissolved, continue to stir under the conditions of 25 DEG C
12min.It weighs seven chloride hydrate cerium of 3g and is added in 15mL deionized water and stir to being completely dissolved labeled as No. 1, then weigh 1g
It is number that seven chloride hydrate ceriums, which are dissolved in label in 15mL deionized water,.Using acid buret by No. 1 solution according to the speed of 1d/s
Degree is added drop-wise to dropwise just in the citric acid solution of cooling and stirring, continues to be stirred to react 10min after being added dropwise.Then it precipitates molten
Liquid is aged 8h under the conditions of 25 DEG C, is filtered under diminished pressure, and adopts and dries 3h after being washed with deionized under the conditions of 70 DEG C, is placed in Muffle furnace
In roast at 500 DEG C after 4h up to amphipathic rod-like nano cerium oxide.
Amphipathic rod-like nano cerium oxide is put into No. 2 solution, 8h is stirred by ultrasonic, up to amphipathic after filtering, drying
Rodlike CeO2/Ce3+Reactive nanoparticles.
Embodiment 3
It weighs 1.5g sodium citrate to be added in 20mL deionized water, is stirred well to and is completely dissolved, continue to stir under the conditions of 0 DEG C
Mix 10min.It weighs six nitric hydrate cerium of 2.17g and is added in 15mL deionized water and stir to being completely dissolved labeled as No. 1, then claim
Taking six nitric hydrate cerium of 1.96g to be dissolved in label in 15mL deionized water is number.Cerous nitrate solution is pressed using acid buret
It is added drop-wise to just in the sodium citrate solution of cooling and stirring dropwise according to the speed of 0.5d/s, continues to be stirred to react after being added dropwise
10min.Then precipitation solution is aged 6h under the conditions of 0 DEG C, is filtered under diminished pressure, and adopts and does under the conditions of 80 DEG C after being washed with deionized
Dry 2h is placed in Muffle furnace at 500 DEG C after roasting 2h up to amphipathic rod-like nano cerium oxide.
Rod-like nano cerium oxide is put into No. 2 solution, 2h is stirred by ultrasonic, up to amphipathic rodlike after filtering, drying
CeO2/Ce3+Reactive nanoparticles.
Embodiment 4
It weighs 2g potassium citrate to be added in 20mL deionized water, is stirred well to and is completely dissolved, continue to stir under the conditions of 10 DEG C
Mix 12min.It weighs tetra- cerium sulfate hydrate of 2g and is added in 15mL deionized water and stir to being completely dissolved labeled as No. 1, then weigh
It is number that tetra- cerium sulfate hydrate of 1.5g, which is dissolved in label in 15mL deionized water,.Using acid buret by cerous nitrate solution according to
The speed of 2d/s is added drop-wise to dropwise just in the potassium citrate solution of cooling and stirring, continues to be stirred to react 15min after being added dropwise.
Then precipitation solution is aged 10h under the conditions of 10 DEG C, is filtered under diminished pressure, and adopts dry under the conditions of 90 DEG C after being washed with deionized
1.5h is placed in Muffle furnace at 550 DEG C after roasting 2h up to amphipathic rod-like nano cerium oxide.
Rod-like nano cerium oxide is put into No. 2 solution, 5h is stirred by ultrasonic, up to amphipathic rodlike after filtering, drying
CeO2/Ce3+Reactive nanoparticles.
Embodiment described above is only to express embodiments of the present invention, and the description thereof is more specific and detailed, but can not
Therefore limitations on the scope of the patent of the present invention are interpreted as.It should be pointed out that those skilled in the art,
Under the premise of not departing from present inventive concept, several deformations, same replacement can also be made, improved etc., these belong to the present invention
Protection scope.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of preparation method of amphipathic rod-like nano cerium oxide, comprising:
Prepare guiding agent aqueous solution and cerous salt aqueous solution；
The guiding agent aqueous solution is mixed and the cerous salt aqueous solution obtains suspension；
The still aging suspension obtains sediment；
Washing, it is dry, roast the sediment and obtain the amphipathic rod-like nano cerium oxide.
2. the preparation method of amphipathic rod-like nano cerium oxide according to claim 1, it is characterised in that:
The guiding agent is citric acid or citrate.
3. the preparation method of amphipathic rod-like nano cerium oxide according to claim 1, it is characterised in that:
The cerous salt is one of cerous nitrate, cerous sulfate or cerium chloride.
4. the preparation method of amphipathic rod-like nano cerium oxide according to claim 1, it is characterised in that:
The molar ratio of the guiding agent and the cerous salt is 1:5 ~ 5:1.
5. the preparation method of amphipathic rod-like nano cerium oxide according to claim 1, it is characterised in that:
The concentration of the guiding agent aqueous solution is 0.03 ~ 4 mol/L；
The concentration of the cerous salt aqueous solution is 0.04 ~ 5mol/L.
6. the preparation method of amphipathic rod-like nano cerium oxide according to claim 1, it is characterised in that:
The mixing guiding agent aqueous solution and the cerous salt aqueous solution, are at 0 ~ 50 DEG C and to be stirred continuously condition
Under, in Xiang Suoshu guiding agent aqueous solution, the cerous salt aqueous solution is added dropwise according to the speed of 0.5 ~ 3d/s, is added dropwise subsequent
0 ~ 10 h of continuous stirring.
7. the preparation method of amphipathic rod-like nano cerium oxide according to claim 1, it is characterised in that:
The washing, using distilled water；The temperature of the drying is 60 ~ 100 DEG C, the time is 2 ~ 8h；The temperature of the roasting is
400 ~ 550 DEG C, the time be 2 ~ 12h.
8. the preparation method of amphipathic rod-like nano cerium oxide according to claim 5, which is characterized in that the guiding agent
Aqueous solution, preparation method are as follows:
It takes the guiding agent in container and adds water, continue ultrasonic disperse, stirring and dissolving obtains the guiding agent aqueous solution.
9. the preparation method of amphipathic rod-like nano cerium oxide according to claim 5, which is characterized in that the trivalent cerium
Saline solution, preparation method are as follows:
It takes the cerous salt in container and adds water, continue ultrasonic disperse, stirring and dissolving obtains the cerous salt aqueous solution.
10. a kind of amphipathic rodlike CeO2/Ce3+The preparation method of reactive nanoparticles, comprising:
The amphipathic rod-like nano cerium oxide is put into the second cerous salt aqueous solution and is stirred, the second precipitating is obtained by filtration
Object；
Dry second sediment obtains the amphipathic rodlike CeO2/Ce3+Reactive nanoparticles.
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