CN103387257B - Method for preparing nano cerium dioxide material by utilizing tween-80 as surfactant - Google Patents
Method for preparing nano cerium dioxide material by utilizing tween-80 as surfactant Download PDFInfo
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- CN103387257B CN103387257B CN201310307042.5A CN201310307042A CN103387257B CN 103387257 B CN103387257 B CN 103387257B CN 201310307042 A CN201310307042 A CN 201310307042A CN 103387257 B CN103387257 B CN 103387257B
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- deionized water
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Abstract
The invention relates to a method for preparing a nano cerium dioxide material by utilizing tween-80 as a surfactant. The method comprises (1) a step of dissolving Ce(NO3)[3] 6H2O in deionized water to obtain a solution A, dissolving sodium oleate and the tween-80 in deionized water to obtain a solution B, mixing the solution A and the solution B, adding cyclohexane, and reacting at 38-40 DEG C to obtain an oil-soluble cerium precursor; (2) a step of dissolving sodium hydroxide in deionized water, and stirring uniformly to obtain a hydroxyl precursor; and (3) a step of adding the hydroxyl precursor into the oil-soluble cerium precursor, stirring to obtain a liquid precursor, then reacting at 170-190 DEG C, and finally separating, washing and drying. The method is simple, and good in repeatability. The method can be produced in a large scale with low cost. Oil-soluble cerium dioxide ultra fine powder prepared by the method has uniform particle size distribution, good dispersibility, and a good application prospect.
Description
Technical field
The invention belongs to nano ceric oxide Material Field, particularly a kind of take tween-80 as the method that nanometer titanium dioxide cerium material prepared by tensio-active agent.
Background technology
As a kind of novel functional materials, nano ceric oxide is widely used as catalytic material, uv-absorbing agent, polishing powder.The performance of nano ceric oxide and its structure, pattern, size and distribution of sizes and the residing chemical physics environment of material itself closely related, these character can by adopting different synthetic methods to regulate and control.Thus, study the controlled synthesis technology of nano ceric oxide, explore differential responses conditions under the coring and increment mechanism of nano ceric oxide significant.
The method preparing nanometer titanium dioxide cerium material conventional at present mainly contains the precipitator method and microemulsion method.Although the precipitator method are easy to operate, the nano particle of preparation is easily reunited, and will carry out roasting and just can obtain nano ceric oxide.The nano material of microemulsion method synthesis has a lot of excellent character, but the method institute in preparation process consumes tensio-active agent and quantity of solvent is more, very difficultly removes these organism and cost is high from particle surface.
Summary of the invention
It take tween-80 as the method that nanometer titanium dioxide cerium material prepared by tensio-active agent that technical problem to be solved by this invention is to provide a kind of, the method is simple and convenient, reproducible, temperature requirement is low, can produce in a large number, cost is low, prepare excellent oil-soluble cerium dioxide ultrafine powder even particle size distribution, good dispersity, has a good application prospect.
Of the present invention a kind of be the method that nanometer titanium dioxide cerium material prepared by tensio-active agent with tween-80, comprising:
(1) by Ce (NO
3)
3.6H
2o dissolves in deionized water, obtains solution A; Sodium oleate and tween-80 are dissolved in deionized water, obtains solution B; By solution A and solution B mixing, then add hexanaphthene, be obtained by reacting oil-soluble cerium precursor in 38-40 DEG C;
(2) sodium hydroxide is dissolved in deionized water, stir and obtain hydroxide radical presoma;
(3) above-mentioned hydroxide radical presoma is joined in above-mentioned oil-soluble cerium precursor, make the volume ratio of oil phase and aqueous phase be 1:1, stir at 38-40 DEG C of lower magnetic force, obtain precursor liquid, then in 170-190 DEG C of reaction 24-28h, last separating, washing, drying.
Ce (NO in solution A described in step (1)
3)
3.6H
2the concentration of O is 0.5M.
In solution B described in step (1), the concentration of sodium oleate is 0.75M, and the amount ratio of tween-80 and deionized water is 0.995-5.953mL:10mL.
In hydroxide radical presoma described in step (2), the concentration of sodium hydroxide is 1M.
The speed that adds of the hydroxide radical presoma described in step (3) is 160mL/h.
Separating, washing described in step (3) is specially after product separation, dehydrated alcohol is added in the oil phase obtained, precipitated in a large number, then centrifugation 10min under 8000rmp, again will the precipitation that obtain successively with deionized water and dehydrated alcohol alternately washing, last ultrasonic disperse and centrifugal.
Drying described in step (3) is at 50 DEG C of dry 12h.
Water-oil interface method refers to that the raw material of reactant is in oil phase and aqueous phase respectively, forms the fabulous lipophilic nano particle of the less homogeneity of particle diameter under lesser temps at oil-water interface; Then nanoparticle enters oil phase under the effect of tensio-active agent, and good dispersity also can steady in a long-termly be preserved in oil phase.Water-oil interface method has reaction conditions gentleness, simple to operate, size tunable, and product purity is high, and productive rate is high, good crystallinity, good dispersity, and particle diameter is little, and cost is low, the advantage that efficiency is high.Oil-soluble nano ceric oxide can be directly used in coating and makeup, is used as uv-absorbing agent, thus decreases and carry out surface modification by water-soluble nano cerium dioxide and obtain the step of oil solubility nanometer cerium dioxide.
Beneficial effect:
(1) the present invention is simple to operate, reaction conditions is gentle, and experimental raw is cheap, good economy performance, can large batch ofly produce;
(2) nano ceric oxide obtained is uniformly dispersed, stable, has a good application prospect.
Accompanying drawing explanation
Fig. 1 is that the water-oil interface legal system of tensio-active agent is for the process flow sheet of nano ceric oxide with tween-80;
Fig. 2 is that the water-oil interface legal system of tensio-active agent is for nano ceric oxide X-ray diffractogram with tween-80;
Fig. 3 is the transmission electron microscope picture of embodiment 1 products therefrom;
Fig. 4 is the transmission electron microscope picture of embodiment 2 products therefrom;
Fig. 5 is the transmission electron microscope picture of embodiment 3 products therefrom.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
(1) 2.2834g(0.0075mol is taken) sodium oleate and 2.976ml(0.0075mol) tween-80 is dissolved completely in 10ml deionized water at 40 DEG C, takes 1.0855g(0.0025mol) Ce (NO
3)
3.6H
2o is dissolved completely in 5ml deionized water, and the two mixes and adds 25ml hexanaphthene, magnetic agitation 0.5h, saves backup;
(2) 0.4g(0.01mol is taken) sodium hydroxide, be dissolved in 10ml deionized water at normal temperatures, magnetic agitation is even, saves backup;
(3) sodium hydroxide step (2) prepared is added drop-wise in the cerium precursor solution of step 1 preparation with the speed of 160ml/h, and the volume ratio stirring 10h(oil phases and aqueous phase at 40 DEG C of lower magnetic forces is 1:1), obtain precursor liquid; The precursor liquid obtained is transferred in reactor, 180 DEG C of reaction 24h, stopped reaction, naturally cool to room temperature, be separated with separating funnel and obtain oil phase, add dehydrated alcohol and produce a large amount of precipitation, the centrifugal 10min of 8000rmp, deionized water and dehydrated alcohol replace washing 3 times, and last 50 DEG C of dry 12h obtain product.
Embodiment 2
(1) 2.2834g(0.0075mol is taken) sodium oleate, 5.953ml(0.015mol) tween-80 is dissolved completely in 10ml deionized water at 40 DEG C, takes 1.0855g(0.0025mol) Ce (NO
3)
3.6H
2o is dissolved completely in 5ml deionized water, and the two mixes and adds 25ml hexanaphthene, magnetic agitation 0.5h, saves backup;
(2) 0.4g(0.01mol is taken) sodium hydroxide, be dissolved in 10ml deionized water at normal temperatures, magnetic agitation is even, saves backup;
(3) sodium hydroxide step (2) prepared is added drop-wise in the cerium precursor solution of step 1 preparation with the speed of 160ml/h, and the volume ratio stirring 10h(oil phases and aqueous phase at 40 DEG C of lower magnetic forces is 1:1), obtain precursor liquid.The precursor liquid obtained is transferred in reactor, 180 DEG C of reaction 24h, stopped reaction, naturally cool to room temperature, be separated with separating funnel and obtain oil phase, add dehydrated alcohol and produce a large amount of precipitation, the centrifugal 10min of 8000rmp, deionized water and dehydrated alcohol replace washing 3 times, and last 50 DEG C of dry 12h obtain product.
Embodiment 3
(1) 2.2834g(0.0075mol is taken) sodium oleate, 0.995ml(0.0025mol) tween-80 is dissolved completely in 10ml deionized water at 40 DEG C, takes 1.0855gCe (NO
3)
3.6H
2o is dissolved completely in 5ml deionized water, and the two mixes and adds 25ml hexanaphthene, magnetic agitation 0.5h, saves backup;
(2) 0.4g(0.01mol is taken) sodium hydroxide, be dissolved in 10ml deionized water at normal temperatures, magnetic agitation is even, saves backup;
(3) sodium hydroxide step (2) prepared is added drop-wise in the cerium precursor solution of step 1 preparation with the speed of 160ml/h, and the volume ratio stirring 10h(oil phases and aqueous phase at 40 DEG C of lower magnetic forces is 1:1), obtain precursor liquid.The precursor liquid obtained is transferred in reactor, 180 DEG C of reaction 24h, stopped reaction, naturally cool to room temperature, be separated with separating funnel and obtain oil phase, add dehydrated alcohol and produce a large amount of precipitation, the centrifugal 10min of 8000rmp, deionized water and dehydrated alcohol replace washing 3 times, and last 50 DEG C of dry 12h obtain product.
Claims (7)
1. be the method that nanometer titanium dioxide cerium material prepared by tensio-active agent with tween-80, comprise:
(1) by Ce (NO
3)
3.6H
2o dissolves in deionized water, obtains solution A; Sodium oleate and tween-80 are dissolved in deionized water, obtains solution B; By solution A and solution B mixing, then add hexanaphthene, be obtained by reacting oil-soluble cerium precursor in 38-40 DEG C;
(2) sodium hydroxide is dissolved in deionized water, stir and obtain hydroxide radical presoma;
(3) above-mentioned hydroxide radical presoma is joined in above-mentioned oil-soluble cerium precursor, make the volume ratio of oil phase and aqueous phase be 1:1, stir at 38-40 DEG C of lower magnetic force, obtain precursor liquid, then in 170-190 DEG C of reaction 24-28h, last separating, washing, drying.
2. according to claim 1 a kind of be the method that nanometer titanium dioxide cerium material prepared by tensio-active agent with tween-80, it is characterized in that: Ce (NO in the solution A described in step (1)
3)
3.6H
2the concentration of O is 0.5M.
3. according to claim 1 a kind of take tween-80 as the method that nanometer titanium dioxide cerium material prepared by tensio-active agent, it is characterized in that: in the solution B described in step (1), the concentration of sodium oleate is 0.75M, the amount ratio of tween-80 and deionized water is 0.995-5.953mL:10mL.
4. according to claim 1 a kind of be the method that nanometer titanium dioxide cerium material prepared by tensio-active agent with tween-80, it is characterized in that: in the hydroxide radical presoma described in step (2), the concentration of sodium hydroxide is 1M.
5. according to claim 1 a kind of be the method that nanometer titanium dioxide cerium material prepared by tensio-active agent with tween-80, it is characterized in that: the speed that adds of the hydroxide radical presoma described in step (3) is 160mL/h.
6. according to claim 1 a kind of take tween-80 as the method that nanometer titanium dioxide cerium material prepared by tensio-active agent, it is characterized in that: the separating, washing described in step (3) is specially after product separation, dehydrated alcohol is added in the oil phase obtained, precipitated in a large number, then centrifugation 10min under 8000rmp, again will the precipitation that obtain successively with deionized water and dehydrated alcohol alternately washing, last ultrasonic disperse and centrifugal.
7. according to claim 1 a kind of be the method that nanometer titanium dioxide cerium material prepared by tensio-active agent with tween-80, it is characterized in that: the drying described in step (3) is at 50 DEG C of dry 12h.
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| CN103754922B (en) * | 2014-01-03 | 2015-08-12 | 东华大学 | A kind of take CTAB as the method that oil solubility nanometer cerium dioxide fluorescent material prepared by tensio-active agent |
| CN105668606B (en) * | 2016-03-11 | 2017-05-31 | 九江学院 | A kind of preparation method of square nano-sheet cerium oxide |
| CN106981572B (en) * | 2017-02-27 | 2019-03-08 | 华中科技大学 | It is a kind of to prepare the modified CeO in surface2The method and product of nano material and application |
| CN108585017A (en) * | 2018-07-24 | 2018-09-28 | 中铝稀土（江苏）有限公司 | A kind of preparation method of rare earth oxide ceria |
| CN111434380B (en) * | 2019-01-11 | 2021-12-21 | 北京化工大学 | Preparation method and application of oil-soluble monodisperse metal oxide nano catalyst |
| CN111662764A (en) * | 2020-06-10 | 2020-09-15 | 江苏凯瑞德润滑技术有限公司 | Method for preparing calcium-based lubricating grease by using waste rapeseed oil and triazine-modified lanthanum oxide |
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| CN101538061A (en) * | 2009-05-06 | 2009-09-23 | 北京化工大学 | Method for preparing nano cerium dioxide |
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| CN101538061A (en) * | 2009-05-06 | 2009-09-23 | 北京化工大学 | Method for preparing nano cerium dioxide |
Non-Patent Citations (2)
| Title |
|---|
| 反相单微乳液法制备纳米二氧化铈及其形貌和分散性研究;范方强等;《无机盐工业》;20090331;第41卷(第3期);第22-24，62页 * |
| 用微乳液法制备CeO2纳米粒子;田中青等;《重庆工学院学报(自然科学版)》;20070831;第21卷(第8期);第75-77，94页 * |
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