CN101638524B - Method for preparing surface-modified nanometer yttrium oxide by emulsion polymerization and application thereof - Google Patents
Method for preparing surface-modified nanometer yttrium oxide by emulsion polymerization and application thereof Download PDFInfo
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- CN101638524B CN101638524B CN2009100420628A CN200910042062A CN101638524B CN 101638524 B CN101638524 B CN 101638524B CN 2009100420628 A CN2009100420628 A CN 2009100420628A CN 200910042062 A CN200910042062 A CN 200910042062A CN 101638524 B CN101638524 B CN 101638524B
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- nanometer yttrium
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Abstract
The invention discloses a method for preparing surface-modified nanometer yttrium oxide by emulsion polymerization and an application thereof. The preparation method has the following steps of: first, preparing nanometer yttrium oxide suspension, adding emulsifier dodecyl trimethyl ammonium chloride, ultrasonically processing, stirring and diffusing for 3h; then, heating to 60 DEG C in nitrogen atmosphere, adding monomer styrene and butyl acrylate with a fixed quality ratio, and finally adding initiator ammonium persulphate to initiate polymerization reaction at 75 DEG C; drying the compound particles obtained after the finishing of the polymerization reaction to obtain the surface-modified nanometer yttrium oxide; and directly ultrasonically diffusing the modified nanometer yttrium oxide in liquid paraffin base oil or finished lubricant as an extreme-pressure, wear-resistant and anti-friction additive. The surface-modified nanometer yttrium oxide has excellent extreme-pressure, wear-resistant and anti-friction effects.
Description
Technical field
The present invention relates to a kind of extreme pressure, wear-resistant, antifriction oil dope, specifically relate to a kind of preparation method of surface-modified nanometer yttrium oxide by emulsion polymerization and as the application of extreme pressure, wear-resistant, antifriction additive.
Background technology
In recent years, nanoparticle has caused many investigators' attention as the research of extreme-pressure anti-wear antifriction additive, and nanoparticle demonstrates excellent tribological property under lubricating condition such as high temperature, high-load, environmental friendliness.But in preparation, there is a drawback, promptly prepares nanoparticle earlier, add suitable dispersion agent then, make it in base oil, form suspension-s.And exposed nanoparticle is grown up owing to high surface energy is prone to coalescence, surfactivity decline, have influence on and dispersion agent between interaction, be unfavorable for stable suspersion.A little less than the reactive force between nanoparticle and the dispersion agent, store with use in cause dispersion agent desorb from the nano-particle surface easily, influence dispersion stabilization and tribological property, greatly limitations its application and popularization as oil dope.
The nano rare earth compound also receives publicity in the applied research of tribological field day by day; The research of nano rare earth compound in tribology at present has been penetrated into numerous areas such as wear-resistant metal material, wear-resisting macromolecular material, wear-resisting pottery; Research as oil dope also has report; Comprise rare earth halide (Tribology International.2001,34:83; Lubricated and sealing, 2006, (12): 37), rare earth oxide (Journal of Shanghai Maritime University.2007,27 (1): 68; Journal of RareEarths.2006,163), (the tribology journal, 2000,20 (3): broad variety nano rare earth compound exhibits goes out good extreme-pressure anti-wear antifriction performance to boric acid rare earth 220) etc. 26 (2):.
Based on the present situation of present research, obtain the high perofmrnace lubricating oils additive, must overcome nanoparticle and very easily reunite and non-oil-soluble shortcoming, therefore develop inorganic-organic nanocomposite compound rare earth based additive and just have great importance.The utilization emulsion polymerization coats one layer of polymeric on nano rare earth inorganics surface; Obtain the advantage that oil-soluble rare earth inorganic-organic nanocomposite has nano material, rare earth material and organic materials concurrently, it is all had bright development prospect as extreme pressure, wear-resistant, the resonable application facet of touching upon of antifriction additive.
Summary of the invention
The purpose of this invention is to provide a kind of rare earth based extreme pressure through the emulsion polymerisation process surface-treated, wear-resistant, antifriction additive specifically is a kind of surface-modified nanometer yttrium oxide by emulsion polymerization.
The preparing method's of a kind of surface-modified nanometer yttrium oxide by emulsion polymerization provided by the invention step is following: at first dispose nano yttrium oxide suspension-s, add the emulsifying agent DTAC, ultrasonic, dispersed with stirring 3h; Under nitrogen atmosphere, be warming up to 60 ℃ then, then add the monomer styrene and the Bing Xisuandingzhi of fixed mass ratio, add initiator ammonium persulfate at last, at 75 ℃ of following initiated polymerizations; The composite particles that polyreaction obtains after finishing is again through being drying to obtain surface-modified nanometer yttrium oxide.
Above-mentioned used nano yttrium oxide particle grain size is between 10~50nm.
The mass ratio of above-mentioned monomer styrene and Bing Xisuandingzhi is 7: 3, and the monomer styrene consumption is 4~14 times of yttrium oxide quality, and the initiator ammonium persulfate consumption is 1%~3% of a monomer styrene quality, and the time of polyreaction is 4~14h.
The surface-modified nanometer yttrium oxide that uses preparation method of the present invention preparation as extreme pressure, wear-resistant, antifriction additive directly through ultra-sonic dispersion in liquid paraffin base oil, perhaps in the finished lube.
The surface-modified nanometer yttrium oxide that uses preparing method's preparation of the present invention is in liquid paraffin base oil, and perhaps the interpolation massfraction in the finished lube is 0.02%~0.5%.
The invention has the beneficial effects as follows: adopt emulsion polymerization to coat one layer of polymeric on the nano yttrium oxide surface; Obtain oil-soluble rare earth inorganic-organic nanocomposite overcome conventional nanoparticle very easily reunite with non-oil-soluble shortcoming; Make it can the long period in stable dispersion in base oil, and shown good extreme pressure, wear-resistant, friction reducing effect.
Description of drawings
Fig. 1 is the XRD figure of the nano yttrium oxide of (b) behind pure nano yttrium oxide (a) and the emulsion polymerizing modification.
Fig. 2, Fig. 3 are the lubricated steel ball mill spot pattern SEM figure down of pure base oil.
Fig. 4, Fig. 5 are the lubricated steel ball mill spot pattern SEM figure down of base oil that adds the nano yttrium oxide of modification.
Embodiment
Embodiment 1:
Take by weighing the nano yttrium oxide 4.35g configuration suspension-s of particle diameter between 10~50nm, add the emulsifying agent DTAC, ultrasonic, dispersed with stirring 3h.Under nitrogen atmosphere, be warming up to 60 ℃ then; Then add the fixed mass ratio and be 7: 3 monomer styrene and Bing Xisuandingzhi; The monomer styrene consumption is 20g, and the initiator ammonium persulfate consumption is 1.5% of a monomer styrene consumption, at 75 ℃ of following initiated polymerization 10h.The composite particles that polyreaction obtains after finishing is again through being drying to obtain surface-modified nanometer yttrium oxide.
Embodiment 2:
Take by weighing the nano yttrium oxide 4.35g configuration suspension-s of particle diameter between 10~50nm, add the emulsifying agent DTAC, ultrasonic, dispersed with stirring 3h.Under nitrogen atmosphere, be warming up to 60 ℃ then; Then add the fixed mass ratio and be 7: 3 monomer styrene and Bing Xisuandingzhi; The monomer styrene consumption is 40g, and the initiator ammonium persulfate consumption is 1.5% of a monomer styrene consumption, at 75 ℃ of following initiated polymerization 10h.The composite particles that polyreaction obtains after finishing is again through being drying to obtain surface-modified nanometer yttrium oxide.
Embodiment 3:
Take by weighing the nano yttrium oxide 4.35g configuration suspension-s of particle diameter between 10~50nm, add the emulsifying agent DTAC, ultrasonic, dispersed with stirring 3h.Under nitrogen atmosphere, be warming up to 60 ℃ then; Then add the fixed mass ratio and be 7: 3 monomer styrene and Bing Xisuandingzhi; The monomer styrene consumption is 60g, and the initiator ammonium persulfate consumption is 1.5% of a monomer styrene consumption, at 75 ℃ of following initiated polymerization 6h.The composite particles that polyreaction obtains after finishing is again through being drying to obtain surface-modified nanometer yttrium oxide.
Embodiment 4:
Take by weighing the nano yttrium oxide 4.35g configuration suspension-s of particle diameter between 10~50nm, add the emulsifying agent DTAC, ultrasonic, dispersed with stirring 3h.Under nitrogen atmosphere, be warming up to 60 ℃ then; Then add the fixed mass ratio and be 7: 3 monomer styrene and Bing Xisuandingzhi; The monomer styrene consumption is 40g, and the initiator ammonium persulfate consumption is 1% of a monomer styrene consumption, at 75 ℃ of following initiated polymerization 4h.The composite particles that polyreaction obtains after finishing is again through being drying to obtain surface-modified nanometer yttrium oxide.
Embodiment 5:
Take by weighing the nano yttrium oxide 4.35g configuration suspension-s of particle diameter between 10~50nm, add the emulsifying agent DTAC, ultrasonic, dispersed with stirring 3h.Under nitrogen atmosphere, be warming up to 60 ℃ then; Then add the fixed mass ratio and be 7: 3 monomer styrene and Bing Xisuandingzhi; The monomer styrene consumption is 40g, and the initiator ammonium persulfate consumption is 3% of a monomer styrene consumption, at 75 ℃ of following initiated polymerization 14h.The composite particles that polyreaction obtains after finishing is again through being drying to obtain surface-modified nanometer yttrium oxide.
Embodiment 6:
Take by weighing the nano yttrium oxide 4.35g configuration suspension-s of particle diameter between 10~50nm, add the emulsifying agent DTAC, ultrasonic, dispersed with stirring 3h.Under nitrogen atmosphere, be warming up to 60 ℃ then; Then add the fixed mass ratio and be 7: 3 monomer styrene and Bing Xisuandingzhi; The monomer styrene consumption is 40g, and the initiator ammonium persulfate consumption is 1% of a monomer styrene consumption, at 75 ℃ of following initiated polymerization 8h.The composite particles that polyreaction obtains after finishing is again through being drying to obtain surface-modified nanometer yttrium oxide.
Embodiment 7:
Nano yttrium oxide after the modification is distributed in liquid paraffin base oil through behind the ultra-sonic dispersion; Perhaps in the finished lube; The massfraction that adds the nano yttrium oxide of modification is 0.02%~0.5% of liquid paraffin base oil or a finished lube quality; And carry out four ball experimental performances and test result such as following table:
Last table content shows that the nano yttrium oxide after the adding letex polymerization surface-treated is as the extreme-pressure anti-wear antifriction additive, and the abrasion resistance of base oil and supporting capacity have raising largely.
Claims (3)
1. the preparation method of a surface-modified nanometer yttrium oxide by emulsion polymerization is characterized in that this preparing method's step is following: at first dispose nano yttrium oxide suspension-s, add the emulsifying agent DTAC, ultrasonic, dispersed with stirring 3h; Under nitrogen atmosphere, be warming up to 60 ℃ then, then add the monomer styrene and the Bing Xisuandingzhi of fixed mass ratio, add initiator ammonium persulfate at last, at 75 ℃ of following initiated polymerizations; The composite particles that polyreaction obtains after finishing is again through being drying to obtain surface-modified nanometer yttrium oxide;
The mass ratio of above-mentioned monomer styrene and Bing Xisuandingzhi is 7: 3, and the monomer styrene consumption is 4~14 times of yttrium oxide quality, and the initiator ammonium persulfate consumption is 1%~3% of a monomer styrene quality, and the time of polyreaction is 4~14h.
2. preparation method according to claim 1 is characterized in that: above-mentioned used nano yttrium oxide particle grain size is between 10~50nm.
3. the surface-modified nanometer yttrium oxide that uses claim 1 preparation method preparation as extreme pressure, wear-resistant, antifriction additive directly through ultra-sonic dispersion in liquid paraffin base oil, perhaps in the finished lube;
Above-mentioned surface-modified nanometer yttrium oxide is in liquid paraffin base oil, and perhaps the interpolation massfraction in the finished lube is 0.02%~0.5%.
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CN101955836B (en) * | 2010-09-26 | 2013-10-09 | 广东工业大学 | Quasi-spherical nano rare earth oxide lubricating oil additive and preparation method thereof |
CN102504146A (en) * | 2011-11-18 | 2012-06-20 | 广东工业大学 | Preparation method and application of coupled modified nanometer yttrium oxide |
CN110655099B (en) * | 2019-11-01 | 2022-05-03 | 常州市卓群纳米新材料有限公司 | Submicron yttrium oxide with high specific surface area and preparation method thereof |
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CN101037218A (en) * | 2007-04-18 | 2007-09-19 | 东北电力大学 | Super hydrophobic yttria powder material having micro-nano structure on surface and preparation method thereof |
CN101260299A (en) * | 2008-04-03 | 2008-09-10 | 沈阳化工学院 | Method for preparing yttrium gadolinium oxide and europium nano luminescent powder by micro-emulsion method |
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CN101037218A (en) * | 2007-04-18 | 2007-09-19 | 东北电力大学 | Super hydrophobic yttria powder material having micro-nano structure on surface and preparation method thereof |
CN101260299A (en) * | 2008-04-03 | 2008-09-10 | 沈阳化工学院 | Method for preparing yttrium gadolinium oxide and europium nano luminescent powder by micro-emulsion method |
Non-Patent Citations (1)
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缪飞等.纳米氧化钇的制备与表征.《精细化工》.2009,第26卷(第4期),313-317. * |
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