CN103387257A - 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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- CN103387257A CN103387257A CN2013103070425A CN201310307042A CN103387257A CN 103387257 A CN103387257 A CN 103387257A CN 2013103070425 A CN2013103070425 A CN 2013103070425A CN 201310307042 A CN201310307042 A CN 201310307042A CN 103387257 A CN103387257 A CN 103387257A
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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 the nano ceric oxide Material Field, particularly a kind of method for preparing the nanometer titanium dioxide cerium material take tween-80 as 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 residing chemical physics environment of the performance of nano ceric oxide and its structure, pattern, size and distribution of sizes and material itself is closely related, and these character can regulate and control by adopting different synthetic methods.Thereby under the controlled technology of preparing of research nano ceric oxide, exploration differential responses condition, nucleation and the growth mechanism of nano ceric oxide are significant.
The method for preparing the nanometer titanium dioxide cerium material commonly used mainly contains the precipitator method and microemulsion method at present.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 synthetic nano material of microemulsion method has the character of a lot of excellences, but the method in preparation process institute's tensio-active agent that consumes and quantity of solvent more, very difficult from particle surface remove these organism and cost high.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method for preparing the nanometer titanium dioxide cerium material take tween-80 as tensio-active agent, the method is simple and convenient, good reproducibility, temperature requirement is low, can produce in a large number, cost is low, prepare good oil-soluble cerium dioxide ultrafine powder size distribution even, good dispersity, have a good application prospect.
A kind of method for preparing the nanometer titanium dioxide cerium material take tween-80 as tensio-active agent of the present invention comprises:
(1) with Ce (NO
3)
3.6H
2O is dissolved in deionized water, obtains solution A; Sodium oleate and tween-80 are dissolved in deionized water, obtain solution B; Solution A and solution B are mixed, then add hexanaphthene, in 38-40 ℃ of reaction, obtain oil-soluble cerium precursor;
(2) with dissolution of sodium hydroxide in deionized water, stir and obtain the hydroxide radical presoma;
(3) above-mentioned hydroxide radical presoma is joined in above-mentioned oil-soluble cerium precursor, the volume ratio that makes oil phase and water is 1:1, at 38-40 ℃ of lower magnetic force, stirs, and obtains precursor liquid, then in 170-190 ℃ of reaction 24-28h, last separating, washing, drying get final product.
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, add dehydrated alcohol in the oil phase that obtains, precipitated in a large number, then centrifugation 10min under 8000rmp, the precipitation that will obtain again is successively with deionized water and alternately washing of dehydrated alcohol, last ultra-sonic dispersion and centrifugal.
Drying described in step (3) is at 50 ℃ of dry 12h.
The water-oil interface method refers to that the raw material of reactant is in respectively oil phase and aqueous phase, forms the fabulous lipophilic nano particle of the less homogeneity of particle diameter at oil-water interface under lesser temps; Then nanoparticle enters oil phase under the effect of tensio-active agent, and good dispersity and energy preservation steady in a long-term in oil phase.The water-oil interface method has the reaction conditions gentleness, and is simple to operate, and particle diameter is controlled, and product purity is high, and productive rate is high, good crystallinity, and good dispersity, 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, thereby reduced by the water-soluble nano cerium dioxide, carries out surface modification and obtains 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, and good economy performance can large batch ofly be produced;
(2) nano ceric oxide that obtains is uniformly dispersed, and is stable, has a good application prospect.
Description of drawings
Fig. 1 is the process flow sheet of the standby nano ceric oxide of water-oil interface legal system take tween-80 as tensio-active agent;
Fig. 2 is the standby nano ceric oxide X-ray diffractogram of the water-oil interface legal system take tween-80 as tensio-active agent;
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 therefroms;
Fig. 5 is the transmission electron microscope picture of embodiment 3 products therefroms.
Embodiment
, below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only are not used in and limit the scope of the invention for explanation the present invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
(1) take 2.2834g(0.0075mol) sodium oleate and 2.976ml(0.0075mol) tween-80 is dissolved in the 10ml deionized water fully under 40 ℃, take 1.0855g(0.0025mol) Ce (NO
3)
3.6H
2O is dissolved in the 5ml deionized water fully, both mixes and add the 25ml hexanaphthene, and magnetic agitation 0.5h, save backup;
(2) take 0.4g(0.01mol) sodium hydroxide, be dissolved at normal temperatures in the 10ml deionized water, magnetic agitation is even, saves backup;
(3) speed of the sodium hydroxide of step (2) preparation with 160ml/h is added drop-wise in the cerium precursor solution of step 1 preparation, the volume ratio that stirs 10h(oil phase and water at 40 ℃ of lower magnetic forces is 1:1), obtain precursor liquid; The precursor liquid that obtains is transferred in reactor, 180 ℃ of reaction 24h, stopped reaction, naturally cool to room temperature, separate and obtain oil phase with separating funnel, add dehydrated alcohol to produce a large amount of precipitations, the centrifugal 10min of 8000rmp, deionized water and dehydrated alcohol alternately wash 3 times, and last 50 ℃ of dry 12h obtain product.
Embodiment 2
(1) take 2.2834g(0.0075mol) sodium oleate, 5.953ml(0.015mol) tween-80 is dissolved in the 10ml deionized water fully under 40 ℃, takes 1.0855g(0.0025mol) Ce (NO
3)
3.6H
2O is dissolved in the 5ml deionized water fully, both mixes and add the 25ml hexanaphthene, and magnetic agitation 0.5h, save backup;
(2) take 0.4g(0.01mol) sodium hydroxide, be dissolved at normal temperatures in the 10ml deionized water, magnetic agitation is even, saves backup;
(3) speed of the sodium hydroxide of step (2) preparation with 160ml/h is added drop-wise in the cerium precursor solution of step 1 preparation, the volume ratio that stirs 10h(oil phase and water at 40 ℃ of lower magnetic forces is 1:1), obtain precursor liquid.The precursor liquid that obtains is transferred in reactor, 180 ℃ of reaction 24h, stopped reaction, naturally cool to room temperature, separate and obtain oil phase with separating funnel, add dehydrated alcohol to produce a large amount of precipitations, the centrifugal 10min of 8000rmp, deionized water and dehydrated alcohol alternately wash 3 times, and last 50 ℃ of dry 12h obtain product.
Embodiment 3
(1) take 2.2834g(0.0075mol) sodium oleate, 0.995ml(0.0025mol) tween-80 is dissolved in the 10ml deionized water fully under 40 ℃, takes 1.0855gCe (NO
3)
3.6H
2O is dissolved in the 5ml deionized water fully, both mixes and add the 25ml hexanaphthene, and magnetic agitation 0.5h, save backup;
(2) take 0.4g(0.01mol) sodium hydroxide, be dissolved at normal temperatures in the 10ml deionized water, magnetic agitation is even, saves backup;
(3) speed of the sodium hydroxide of step (2) preparation with 160ml/h is added drop-wise in the cerium precursor solution of step 1 preparation, the volume ratio that stirs 10h(oil phase and water at 40 ℃ of lower magnetic forces is 1:1), obtain precursor liquid.The precursor liquid that obtains is transferred in reactor, 180 ℃ of reaction 24h, stopped reaction, naturally cool to room temperature, separate and obtain oil phase with separating funnel, add dehydrated alcohol to produce a large amount of precipitations, the centrifugal 10min of 8000rmp, deionized water and dehydrated alcohol alternately wash 3 times, and last 50 ℃ of dry 12h obtain product.
Claims (7)
1. method for preparing the nanometer titanium dioxide cerium material take tween-80 as tensio-active agent comprises:
(1) with Ce (NO
3)
3.6H
2O is dissolved in deionized water, obtains solution A; Sodium oleate and tween-80 are dissolved in deionized water, obtain solution B; Solution A and solution B are mixed, then add hexanaphthene, in 38-40 ℃ of reaction, obtain oil-soluble cerium precursor;
(2) with dissolution of sodium hydroxide in deionized water, stir and obtain the hydroxide radical presoma;
(3) above-mentioned hydroxide radical presoma is joined in above-mentioned oil-soluble cerium precursor, the volume ratio that makes oil phase and water is 1:1, at 38-40 ℃ of lower magnetic force, stirs, and obtains precursor liquid, then in 170-190 ℃ of reaction 24-28h, last separating, washing, drying get final product.
2. a kind of method for preparing the nanometer titanium dioxide cerium material take tween-80 as tensio-active agent according to claim 1, 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. a kind of method for preparing the nanometer titanium dioxide cerium material take tween-80 as tensio-active agent according to claim 1, it is characterized in that: in the 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.
4. a kind of method for preparing the nanometer titanium dioxide cerium material take tween-80 as tensio-active agent according to claim 1, it is characterized in that: in the hydroxide radical presoma described in step (2), the concentration of sodium hydroxide is 1M.
5. a kind of method for preparing the nanometer titanium dioxide cerium material take tween-80 as tensio-active agent according to claim 1, it is characterized in that: the speed that adds of the hydroxide radical presoma described in step (3) is 160mL/h.
6. a kind of method for preparing the nanometer titanium dioxide cerium material take tween-80 as tensio-active agent according to claim 1, it is characterized in that: the separating, washing described in step (3) is specially after product separation, add dehydrated alcohol in the oil phase that obtains, precipitated in a large number, then centrifugation 10min under 8000rmp, the precipitation that will obtain again is successively with deionized water and alternately washing of dehydrated alcohol, last ultra-sonic dispersion and centrifugal.
7. a kind of method for preparing the nanometer titanium dioxide cerium material take tween-80 as tensio-active agent according to claim 1 is characterized in that: the drying described in step (3) is at 50 ℃ of dry 12h.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103754922A (en) * | 2014-01-03 | 2014-04-30 | 东华大学 | Method for preparing oil-soluble nano cerium dioxide fluorescent powder by using CTAB (cetyltrimethyl ammonium bromide) as surfactant |
| CN105668606A (en) * | 2016-03-11 | 2016-06-15 | 九江学院 | Preparing method for square nanometer flake cerium oxide |
| CN106981572A (en) * | 2017-02-27 | 2017-07-25 | 华中科技大学 | A kind of CeO for preparing surface modification2The 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 |
| CN111434380A (en) * | 2019-01-11 | 2020-07-21 | 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
|---|
| 田中青等: "用微乳液法制备CeO2纳米粒子", 《重庆工学院学报(自然科学版)》, vol. 21, no. 8, 31 August 2007 (2007-08-31) * |
| 范方强等: "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", 《无机盐工业》, vol. 41, no. 3, 31 March 2009 (2009-03-31) * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103754922A (en) * | 2014-01-03 | 2014-04-30 | 东华大学 | Method for preparing oil-soluble nano cerium dioxide fluorescent powder by using CTAB (cetyltrimethyl ammonium bromide) as surfactant |
| 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 |
| CN105668606A (en) * | 2016-03-11 | 2016-06-15 | 九江学院 | Preparing method for square nanometer flake cerium oxide |
| CN105668606B (en) * | 2016-03-11 | 2017-05-31 | 九江学院 | A kind of preparation method of square nano-sheet cerium oxide |
| CN106981572A (en) * | 2017-02-27 | 2017-07-25 | 华中科技大学 | A kind of CeO for preparing surface modification2The method and product of nano material and application |
| 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 |
| CN111434380A (en) * | 2019-01-11 | 2020-07-21 | 北京化工大学 | Preparation method and application of oil-soluble monodisperse metal oxide nano catalyst |
| 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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