CN109825112A - A kind of perfluorocarboxylic acid modification zinc oxide nanoparticle and its preparation method and application - Google Patents
A kind of perfluorocarboxylic acid modification zinc oxide nanoparticle and its preparation method and application Download PDFInfo
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- CN109825112A CN109825112A CN201910220340.8A CN201910220340A CN109825112A CN 109825112 A CN109825112 A CN 109825112A CN 201910220340 A CN201910220340 A CN 201910220340A CN 109825112 A CN109825112 A CN 109825112A
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- perfluorocarboxylic acid
- zinc oxide
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Abstract
The invention belongs to lubricating oil and grease additive technical field, a kind of perfluorocarboxylic acid modification zinc oxide nanoparticle and its preparation method and application is disclosed.Zinc hydroxide is dissolved in the ethanol solution of perfluorocarboxylic acid, 30-50 DEG C of reaction 2-3 h removes solvent after reaction, and then ice water washing filtering, obtains perfluorocarboxylic acid zinc；Perfluorocarboxylic acid zinc, inorganic strong alkali or organic alkali are dissolved in polar organic solvent, 30 ~ 50 DEG C of 10 ~ 14 h of reaction remove solvent after reaction, are washed out, obtain perfluorocarboxylic acid modification zinc oxide nanoparticle.Perfluorocarboxylic acid modification zinc oxide nanoparticle is in perfluoro polyether oil as the application of antiwear and friction-reducing additive.Preparation method reaction system of the present invention is nontoxic, low temperature, equipment is simple, yield is high, it is suitble to large-scale industrial production, keep prepared perfluorocarboxylic acid modification zinc oxide nanoparticle partial size small by the production method of in-situ modification control growth, uniform particle diameter has good dispersion stabilization in perfluoropolyether class lubricating oil.
Description
Technical field
The invention belongs to lube oil additive technical fields, and in particular to a kind of perfluorocarboxylic acid modification zinc oxide nanoparticle and
Preparation method and application.
Background technique
The Viscosity Index of perfluoropolyether (PFPE) is up to 358, and freezing point is lower than -60 DEG C, and thermal decomposition temperature is 390 DEG C,
Vacuum Heat volatilization loss amount only has 0.21%.Perfluoropolyether high temperature performance excellent in this way and vacuum stability, become one
The space flight lubricant grease that kind can not be substituted.Meanwhile being also applied to all kinds of vacuum pumps, corrosive environment, current-carrying device and core work
Mechanical lubrication field under the various harsh conditions such as industry.But since the strand of perfluoropolyether is made of perfluoro ether chain,
It hardly mixes with any traditional lubricating additive, its anti-wear and wear-resistant performance is caused to be unable to get improvement.Nano zine oxide tool
There are anti-wear and wear-resistant performance outstanding and the repair ability secondary to friction, has in fields such as lubricant grease, lubrication seal rubbers
Extensive purposes.But the unmodified zinc oxide nano grain of rice can not in lubricant grease stable dispersion, thus cannot obtain extensively
Using.The preparation method of oil insoluble oxidation zinc nanoparticle is mainly by being blended ball with organic modifier for Zinc oxide powder at present
It grinds (CN201610929086), or the zinc oxide after ball milling is blended with the lubricant grease containing organic dispersing agent
(CN201610298785；CN201510575435；CN201110452894), it is scattered in Zinc oxide powder in lubricant medium.
Since dressing agent is not engaged in the generation reaction of the zinc oxide nano grain of rice in above method, it can not fundamentally inhibit zinc-oxide nano
The excessive growth and reunion of grain guarantee the long-time stability of its dispersion, and it is even more impossible to so that it is stably dispersed in perfluoropolyether lubrication
In oil, become its antiwear and friction-reducing additive.
Summary of the invention
To overcome the shortcomings of the prior art, the purpose of the present invention is intended to provide a kind of perfluorocarboxylic acid modification oxygen
Change zinc nanoparticle and its preparation method and application.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of preparation method of perfluorocarboxylic acid modification zinc oxide nanoparticle, preparation step are as follows:
(1), zinc hydroxide is dissolved in the ethanol solution of perfluorocarboxylic acid, 30-50 DEG C of reaction 2-3 h is removed after reaction
Solvent is removed, then ice water washing filtering, obtains perfluorocarboxylic acid zinc；
(2), perfluorocarboxylic acid zinc, inorganic strong alkali or organic alkali are dissolved in polar organic solvent, 30 ~ 50 DEG C of reactions 10 ~ 14
H removes solvent after reaction, is washed out, and obtains perfluorocarboxylic acid modification zinc oxide nanoparticle；
Wherein, in step (1), the concentration of the ethanol solution of perfluorocarboxylic acid is 2-4 mol/L, zinc hydroxide and perfluorocarboxylic acid
Molar ratio be (0.5-1): 1；In step (2), perfluorocarboxylic acid zinc: the molar ratio of inorganic strong alkali or organic alkali is (0.5-2):
1, the final concentration of 0.05-0.2 mol/L of inorganic strong alkali or organic alkali in polar organic solvent.
Preferably, the perfluorocarboxylic acid is straight chain perfluoro fatty acid of the carbon atom number between 7 ~ 22, carbon atom number 7
The combination of one or more of branch perfluoro fatty acid between ~ 22.
Preferably, the polar organic solvent is one or more of tetrahydrofuran, dehydrated alcohol, methanol to appoint
The mixed solvent of volume ratio of anticipating composition.
Preferably, the inorganic strong alkali is alkali metal hydroxide or alkaline earth metal hydroxide；The organic alkali is
Tetraalkyl replaces quaternary ammonium base, and wherein alkyl is direct-connected aliphatic hydrocarbon of the carbon atom number between 2 ~ 4.
A kind of perfluorocarboxylic acid modification zinc oxide nanoparticle prepared using the preparation method.
Perfluorocarboxylic acid modification zinc oxide nanoparticle is in perfluoro polyether oil as the application of antiwear and friction-reducing additive.
Preferably, additive amount of the perfluorocarboxylic acid modification zinc oxide nanoparticle in perfluoro polyether oil is 2-5 wt%.
The present invention is during preparing perfluorocarboxylic acid zinc, in order to guarantee the purity of perfluorocarboxylic acid zinc, simplify processing step,
The molar ratio of zinc hydroxide and perfluorocarboxylic acid is (0.5-1): 1；In order to control the partial size of perfluorocarboxylic acid modification zinc oxide nanoparticle
And its dispersion stabilization, dehydration temperature need to control at 30 ~ 50 DEG C, the reaction time controls between 10 ~ 14 h；In order to
Realize that dispersion stabilization of the zinc oxide nano grain of rice in perfluoropolyether class lubricating oil, perfluorocarboxylic acid are carbon atom number between 7 ~ 22
One or more of branch perfluoro fatty acid between 7 ~ 22 of straight chain perfluoro fatty acid, carbon atom number combination.
Preparation method reaction system of the present invention is nontoxic, low temperature, and equipment is simple, yield is high, is suitble to large-scale industrial production, leads to
The production method for crossing in-situ modification control growth keeps prepared perfluorocarboxylic acid modification zinc oxide nanoparticle partial size small, and partial size is equal
One, in perfluoropolyether class lubricating oil have good dispersion stabilization, aviation, vacuum, strong corrosive environment, current-carrying device with
And nuclear industry is had broad application prospects with lube oil additive field.
Detailed description of the invention
Fig. 1: transmission electron microscope (TEM) figure of perfluoro caprylic acid modification zinc oxide nanoparticle made from embodiment 1.
Fig. 2: the X-ray diffraction (XRD) figure of perfluoro caprylic acid modification zinc oxide nanoparticle made from embodiment 1.
Fig. 3: infrared spectrometer (FTIR) figure of perfluoro caprylic acid modification zinc oxide nanoparticle made from embodiment 1.
Fig. 4: the wear rate of perfluoro polyether oil with concentration variation diagram.
Fig. 5: the variation diagram of the coefficient of friction of perfluoro polyether oil at any time.
Specific embodiment
Technical solution of the present invention is further discussed in detail with reference to embodiments, but protection scope of the present invention
It is not limited thereto.
Embodiment 1
A kind of preparation method of perfluoro caprylic acid modification zinc oxide nanoparticle, specifically:
(1), in 25 mL single-necked flasks, the ethanol solution and 12 mmol of the perfluoro caprylic acid of 8 mL, 3 mol/L is added
Zinc hydroxide, 50 DEG C of stirring in water bath react 2 h, and after sample is rotated, ice water washing filtering obtains perfluoro caprylic acid zinc；
(2), sequentially added in 50 mL single-necked flasks 15 mL tetrahydrofurans, upper step preparation 0.8 mmol of perfluoro caprylic acid zinc,
The methanol solution of 0.5 mL, 1.6 mol/L sodium hydroxide reacts 12 h in 50 DEG C of stirring in water bath, after reaction passes through sample
Cross revolving, washing obtains perfluoro caprylic acid modification zinc oxide nanoparticle white powder.
The transmission electron microscope picture of perfluoro caprylic acid modification zinc oxide nanoparticle obtained is shown in Fig. 1.As seen from Figure 1, made
Standby perfluoro caprylic acid modification zinc oxide nanoparticle, uniform particle diameter, are isolated by dressing agent between particle, are not had by 4 nanometers of average grain diameter
There is agglomeration.
The X-ray diffractogram of perfluoro caprylic acid modification zinc oxide nanoparticle obtained is shown in Fig. 2.In figure 31.769 °,
The standard card of diffraction maximum and zinc oxide at 34.421 °, 36.252 °, 47.538 °, 56.602 °, 62.862 °, 67.961 °
(JCPDS card number 36-1451) unanimously, respectively correspond the feature diffraction crystal face (100) of zinc oxide, (002), (101), (102),
(110), (103), (112), and diffraction maximum has significantly broadened phenomenon in figure, it is described above to be successfully prepared the lesser oxygen of partial size
Change zinc nanoparticle.
The infrared spectrogram (FTIR) of perfluoro caprylic acid modification zinc oxide nanoparticle obtained is shown in Fig. 3.It is complete after being modified in figure
Fluorine octanoic acid modification zinc oxide nanoparticle is in 1145cm-1、1210cm-1- CF in the peak position and perfluoro caprylic acid at place2-、-CF3The vibration of key
Peak position is consistent, is located at 3422cm-1Broadening occurs for the absorption peak at place and the stretching vibration peak red shift of C=O is to 1684cm-1,
455cm simultaneously-1There is the vibration peak of Zn-O key in place, and perfluoro caprylic acid modification described above is on ZnO nano grain.
Prepared perfluoro caprylic acid modification zinc oxide nanoparticle is added in perfluoro polyether oil, perfluoro polyether oil
Wear rate is as shown in Figure 4 with the variation diagram of perfluoro caprylic acid modification zinc oxide nanoparticle addition concentration, it is known that addition ZnO nano grain
Afterwards, when addition concentration is 3wt%, there is optimal antifriction performance, wear rate reduces 49.83%.
Further, the variation diagram of the coefficient of friction for the perfluoro polyether oil that addition concentration is 3wt% at any time is shown in Fig. 5.
As seen from Figure 5: after addition ZnO nano grain, the coefficient of friction of perfluoro caprylic acid reduces 2.75%.At the same time, observation is stood
Perfluoro polyether oil 3 months that concentration is 3wt% are added, do not occur Precipitation.
Embodiment 2
A kind of preparation method of perfluoro caprylic acid modification zinc oxide nanoparticle, specifically:
(1), in 25 mL single-necked flasks, the ethanol solution and 12 mmol hydrogen of the perfluoro caprylic acid of 8 mL, 3 mol/L is added
Zinc oxide, 50 DEG C of stirring in water bath react 2 h, and after sample is rotated, ice water washing filtering obtains perfluoro caprylic acid zinc；
(2), sequentially added in 50 mL single-necked flasks 15 mL dehydrated alcohols, upper step preparation 0.8 mmol of perfluoro caprylic acid zinc,
The methanol solution (40 wt%) of 0.52 mL tetrabutylammonium hydroxide solution reacts 12 h in 50 DEG C of stirring in water bath, and reaction terminates
Sample is obtained into perfluoro caprylic acid modification zinc oxide nanoparticle white powder by revolving, washing afterwards.
Embodiment 3
A kind of preparation method of perfluoro-heptanoic acid modification zinc oxide nanoparticle, specifically:
(1), in 25 mL single-necked flasks, the ethanol solution and 12 mmol of the perfluoro-heptanoic acid of 8 mL, 3 mol/L is added
Zinc hydroxide, 50 DEG C of stirring in water bath react 2 h, and after sample is rotated, ice water washing filtering obtains perfluoro-heptanoic acid zinc；
(2), sequentially added in 50 mL single-necked flasks 15 mL tetrahydrofurans, upper step preparation 0.8 mmol of perfluoro-heptanoic acid zinc,
The methanol solution of 0.5 mL, 1.6 mol/L sodium hydroxide reacts 13 h in 40 DEG C of stirring in water bath, after reaction passes through sample
Cross revolving, washing obtains perfluoro-heptanoic acid modification zinc oxide nanoparticle white powder.
Embodiment 4
A kind of preparation method of perfluoro-pelargonic acid modification zinc oxide nanoparticle, specifically:
(1), in 25 mL single-necked flasks, the ethanol solution and 12 mmol of the perfluoro-pelargonic acid of 8 mL, 3 mol/L is added
Zinc hydroxide, 50 DEG C of stirring in water bath react 2 h, and after sample is rotated, ice water washing filtering obtains perfluoro-pelargonic acid zinc；
(2), sequentially added in 50 mL single-necked flasks 15 mL tetrahydrofurans, upper step preparation 0.8 mmol of perfluoro-pelargonic acid zinc,
The methanol solution of 0.5 mL, 1.6 mol/L sodium hydroxide reacts 14 h in 30 DEG C of stirring in water bath, after reaction passes through sample
Cross revolving, washing obtains perfluoro-pelargonic acid modification zinc oxide nanoparticle white powder.
Embodiment 5
A kind of preparation method of perfluoro-heptanoic acid modification zinc oxide nanoparticle, specifically:
(1), in 25 mL single-necked flasks, the ethanol solution and 12 mmol of the perfluoro-heptanoic acid of 8 mL, 3 mol/L is added
Zinc hydroxide, 50 DEG C of stirring in water bath react 2 h, and after sample is rotated, ice water washing filtering obtains perfluoro-heptanoic acid zinc；
(2), sequentially added in 50 mL single-necked flasks 15 mL dehydrated alcohols, upper step preparation 0.8 mmol of perfluoro-heptanoic acid zinc,
The methanol solution (40 wt%) of 0.52 mL tetrabutylammonium hydroxide reacts 10 h in 50 DEG C of stirring in water bath, after reaction will
Sample obtains perfluoro-heptanoic acid modification zinc oxide nanoparticle white powder by revolving, washing.
Embodiment 6
A kind of preparation method of perfluoro-pelargonic acid modification zinc oxide nanoparticle, specifically:
(1), in 25 mL single-necked flasks, the ethanol solution and 12 mmol of the perfluoro-pelargonic acid of 8 mL, 3 mol/L is added
Zinc hydroxide, 50 DEG C of stirring in water bath react 2 h, and after sample is rotated, ice water washing filtering obtains perfluoro-pelargonic acid zinc；
(2), sequentially added in 50 mL single-necked flasks 15 mL dehydrated alcohols, upper step preparation 0.8 mmol of perfluoro-pelargonic acid zinc,
The methanol solution (40 wt%) of 0.52 mL tetrabutylammonium hydroxide reacts 14 h in 30 DEG C of stirring in water bath, after reaction will
Sample obtains perfluoro-pelargonic acid modification zinc oxide nanoparticle white powder by revolving, washing.
Embodiment 7
A kind of preparation method of perfluoro-heptanoic acid modification zinc oxide nanoparticle, specifically:
(1), in 25 mL single-necked flasks, the ethanol solution and 12 mmol of the perfluoro-heptanoic acid of 8 mL, 3 mol/L is added
Zinc hydroxide, 50 DEG C of stirring in water bath react 2 h, and after sample is rotated, ice water washing filtering obtains perfluoro-heptanoic acid zinc；
(2), sequentially added in 50 mL single-necked flasks 15 mL tetrahydrofurans, upper step preparation 0.8 mmol of perfluoro-heptanoic acid zinc,
The methanol solution (40 wt%) of 0.52 mL tetraethyl ammonium hydroxide reacts 10 h in 50 DEG C of stirring in water bath, after reaction will
Sample obtains perfluoro-heptanoic acid modification zinc oxide nanoparticle white powder by revolving, washing.
Embodiment 8
A kind of preparation method of perfluoro caprylic acid modification zinc oxide nanoparticle, specifically:
(1), in 25 mL single-necked flasks, the ethanol solution and 12 mmol of the perfluoro caprylic acid of 8 mL, 3 mol/L is added
Zinc hydroxide, 50 DEG C of stirring in water bath react 2 h, and after sample is rotated, ice water washing filtering obtains perfluoro caprylic acid zinc；
(2), sequentially added in 50 mL single-necked flasks 15 mL dehydrated alcohols, upper step preparation 0.8 mmol of perfluoro caprylic acid zinc,
The methanol solution (40 wt%) of 0.52 mL tetrapropylammonium hydroxide reacts 12 h in 40 DEG C of stirring in water bath, after reaction will
Sample obtains perfluoro caprylic acid zinc oxide nano grain of rice white powder by revolving, washing.
Claims (7)
1. a kind of preparation method of perfluorocarboxylic acid modification zinc oxide nanoparticle, which is characterized in that preparation step is as follows:
(1), zinc hydroxide is dissolved in the ethanol solution of perfluorocarboxylic acid, 30-50 DEG C of reaction 2-3 h is removed after reaction
Solvent is removed, then ice water washing filtering, obtains perfluorocarboxylic acid zinc；
(2), perfluorocarboxylic acid zinc, inorganic strong alkali or organic alkali are dissolved in polar organic solvent, 30 ~ 50 DEG C of reactions 10 ~ 14
H removes solvent after reaction, is washed out, and obtains perfluorocarboxylic acid modification zinc oxide nanoparticle；
Wherein, in step (1), the concentration of the ethanol solution of perfluorocarboxylic acid is 2-4 mol/L, zinc hydroxide and perfluorocarboxylic acid
Molar ratio be (0.5-1): 1；In step (2), perfluorocarboxylic acid zinc: the molar ratio of inorganic strong alkali or organic alkali is (0.5-2):
1, the final concentration of 0.05-0.2 mol/L of inorganic strong alkali or organic alkali in polar organic solvent.
2. the preparation method of perfluorocarboxylic acid modification zinc oxide nanoparticle as described in claim 1, it is characterised in that: the perfluor
Carboxylic acid is straight chain perfluoro fatty acid, carbon atom number branch perfluor fat subsitutes 7 ~ 22 between of the carbon atom number between 7 ~ 22
The combination of one or more of acid.
3. the preparation method of perfluorocarboxylic acid modification zinc oxide nanoparticle as described in claim 1, it is characterised in that: the polarity
Organic solvent be one or more of tetrahydrofuran, dehydrated alcohol, methanol with arbitrary volume than the mixed solvent that forms.
4. the preparation method of perfluorocarboxylic acid modification zinc oxide nanoparticle as described in claim 1, it is characterised in that: described inorganic
Highly basic is alkali metal hydroxide or alkaline earth metal hydroxide；The organic alkali is that tetraalkyl replaces quaternary ammonium base, wherein hydrocarbon
Base is direct-connected aliphatic hydrocarbon of the carbon atom number between 2 ~ 4.
5. a kind of perfluorocarboxylic acid modification zinc oxide nanoparticle prepared such as any preparation method of claim 1 ~ 4.
6. a kind of perfluorocarboxylic acid modification zinc oxide nanoparticle as claimed in claim 5 is used as antifriction in perfluoro polyether oil
The application of antiwear additive.
7. application as claimed in claim 6, it is characterised in that: perfluorocarboxylic acid modification zinc oxide nanoparticle is lubricated in perfluoropolyether
Additive amount in oil is 2-5 wt%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111635804A (en) * | 2019-11-22 | 2020-09-08 | 中国科学院兰州化学物理研究所 | Perfluoropolyether supermolecule gel composite nanoparticle lubricant and preparation method and application thereof |
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