CN108893176A - A kind of perfluoro polyether oil and preparation method thereof - Google Patents
A kind of perfluoro polyether oil and preparation method thereof Download PDFInfo
- Publication number
- CN108893176A CN108893176A CN201810602648.4A CN201810602648A CN108893176A CN 108893176 A CN108893176 A CN 108893176A CN 201810602648 A CN201810602648 A CN 201810602648A CN 108893176 A CN108893176 A CN 108893176A
- Authority
- CN
- China
- Prior art keywords
- integer
- perfluoro polyether
- oil
- perfluoropolyether
- polyether oil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M133/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen
- C10M133/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
- C10M133/38—Heterocyclic nitrogen compounds
- C10M133/44—Five-membered ring containing nitrogen and carbon only
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M133/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen
- C10M133/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M133/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen
- C10M133/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
- C10M133/38—Heterocyclic nitrogen compounds
- C10M133/48—Heterocyclic nitrogen compounds the ring containing both nitrogen and oxygen
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/06—Perfluoro polymers
- C10M2213/0606—Perfluoro polymers used as base material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/08—Amides
- C10M2215/082—Amides containing hydroxyl groups; Alkoxylated derivatives
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/22—Heterocyclic nitrogen compounds
- C10M2215/223—Five-membered rings containing nitrogen and carbon only
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/22—Heterocyclic nitrogen compounds
- C10M2215/225—Heterocyclic nitrogen compounds the rings containing both nitrogen and oxygen
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/10—Inhibition of oxidation, e.g. anti-oxidants
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/12—Gas-turbines
- C10N2040/13—Aircraft turbines
Abstract
The invention discloses a kind of perfluoro polyether oils, consist of the following compositions：90~98wt% of base oil, antioxidant anticorrosive 0.1~5wt% of agent, 0.1~5wt% of antiwear additive.The invention also discloses the preparation methods of the perfluoro polyether oil.The present invention solves the problems, such as that existing perfluoro polyether oil is easy to decompose at high temperature and corrodes metal.
Description
Technical field
The invention belongs to petrochemical industries, and in particular to a kind of aero-turbine perfluoro polyether oil and its system
Preparation Method.
Technical background
Mainly according to the mark that rises to of its thrust ratio, the raising of thrust ratio is mainly for the development of modern Aviation turbogenerator
Temperature before raising engine turbine, the raising of turbine inlet temperature directly affect neighbouring base bearing temperature, eventually lead to engine
Lubricating system temperature is also with improve.High performance aero-turbine needs the comparable lubricating oil of performance phase therewith
Match.The beginning of the eighties in last century, United States Air Force propose to meet alternate-engine work according to the development trend of aero-turbine
It is required that true lubrication oil basic performance indices, the whole lubrication temperature that wherein lubricating oil may be born, i.e., lubrication in fuel tank
The highest stabilizing temperature of oil is 260-427 DEG C, this has had exceeded the high temperature limit that Esters oil can bear.In order to meet future
Demand of the aero-engine to high temperature grease, needs to develop novel high temperature grease
The need that the high temperature grease of various new is used to meet aero-engine for high temperature grease have been developed at present
It asks, such as modified polysiloxanes, polyphenylene oxide, three phosphorus azo of ring.But these synthetic lubricant fluids itself all have many defects,
For example, polymethylphenyl siloxane fluid and trifluoro propyl silicone oil boundary lubrication ability are poor, resisting combustibility is not good enough, is easy to produce intersection in oxidation
Coupling tendency, makes it under identical oxygen absorbed, and viscosity increases above other synthetic lubricant fluids, corrosivity also compared with
By force；Polyphenylene oxide pour point is up to 4 DEG C, when be lower than 15 DEG C under conditions of in use, must be diluted with trichloro ethylene, to limit
Its application is made, in addition its relatively poor greasy property and expensive cost also limit its application；Three phosphorus of limitation ring is even
The greatest problem of nitrogen application is that its production cost is more much higher than other lubricating oil.Therefore develop novel high temperature grease with
It is most important to meet high temperature aviation lubrication needs.
Perfluoropolyether (PFPE) is the polymer in a kind of molecular structure only containing tri- kinds of elements of C, F, O.PFPE molecule knot
Structure and hydro carbons pfpe molecule structure are very similar, but with stronger carbon fluorine (C-F) key instead of hydrocarbon (C-H) key, in molecule with
Fluorine atom is instead of hydrogen atom.C-F key in PFPE molecule has very strong shielding action to main chain, makes it have very high anti-
Oxidisability, chemical inertness, corrosion resistance and radiation resistance；In addition, PFPE also have good viscosity-temperature characteristics, low vapo(u)rability,
Low pour point, preferable thermal stability, the features such as temperature limit is wide；Fluorine ether oil prepared therefrom can apply to harshness
It is a kind of good special lubricating oil under environment.But under high temperature (being greater than 250 DEG C) static environment or in Rough Contact
When local temperature and shear stress are in maximum value in friction environment, perfluoropolyether can with metal reaction and degrade, wherein
A kind of product is PFPE acyl fluorides, and PFPE acyl fluorides can be reacted with metal or stainless steel surface generates metal fluoride (FeF3) Louis
Sour site, the FeF at Lewis-acid sites3Perfluoro polyether oil can be catalyzed to degrade, the acyl fluorides class product of generation can be further
It is acted on metal surface, new Lewis-acid sites is formed, to cause to corrode to metal.To guarantee PFPE lubricating oil in high temperature
Or normal use under the harsh conditions such as Rough Contact, antioxidant anticorrosive agent usually is added and antiwear additive solves the problems, such as this.However often
The additive of rule does not dissolve in perfluoropolyether, can not solve the problems, such as corresponding.
Summary of the invention
To solve the above problems, the present invention is lacked for what perfluoropolyether was decomposed under high temperature and condition of boundary lubrication
It falls into and conventional additives cannot be dissolved in the objective fact of perfluoroether polyethers, design and synthesize out a series of can be dissolved in very well
The additive of perfluoropolyether.These additives be dissolved in after perfluoropolyether can stable metal, prevent from corroding and enhance lubricity (i.e.
Improve wear resistence).These additives can substantially be divided to two classes, i.e. antioxidant anticorrosive agent and antiwear additive.And it is perfluoropolyether basis is oily
It is compounded with antioxidant anticorrosive agent and antiwear additive ratio by weight, mixes a kind of aero-turbine that can be applied to
High temperature grease.
First aspect present invention discloses a kind of perfluoro polyether oil, consists of the following compositions：Base oil 90~
98wt%, antioxidant anticorrosive 0.1~5wt% of agent, 0.1~5wt% of antiwear additive.
Preferably, the base oil is K-type perfluoropolyether or D type perfluoropolyether, the structural formula of the K-type perfluoropolyether
For：The wherein integer that m is 20~50；
The D type perfluoropolyether structures formula：CF3-CF2-CF2-O(CF2-CF2-CF2-O)nCF2CF3, wherein n is 20~50
Integer.
Preferably, the antioxidant anticorrosive agent is the benzotriazole of Rf modification, benzimidazole, benzopyrazoles, benzoxazoles
With one of benzothiazole or a variety of, structural formula is as follows：
The Rf is CxF2x-1-、C3F7O
(CF2CF2CF2O)yCF2CF2Or C3F7O{CF(CF3)CF2O}zCF(CF3)-one or more of, wherein x be 5~15 it is whole
Number, the integer that y is 5~15, the integer that z is 5~15.
Preferably, the antiwear additive is one of Perfluoropolyether amide alcohol or sulfur alcohol compound or a variety of, chemistry
Formula is RfCONH (CH2)pOH or RfCONH (CH2)pSH；The Rf is CxF2x-1-、C3F7O(CF2CF2CF2O)yCF2CF2Or
C3F7O{CF(CF3)CF2O}zCF(CF3One or more of)-, the integer that wherein p is 2~10, the integer that x is 5~15, y is
5~15 integer, the integer that z is 5~15.
Preferably, 40 DEG C of the viscosity of the perfluoro polyether oil when be 100~500mm2/ s, pour point are -30 DEG C~-50
Between DEG C.
Second aspect of the present invention discloses the preparation method of the perfluoro polyether oil, includes the following steps：It will be basic
Oil is heated to 60 DEG C, and antioxidant anticorrosive agent and antiwear additive is added, is warming up to 80 DEG C of 1~2h of mixing, is filtered to remove at this temperature
Filter residue is up to the perfluoro polyether oil.
Preferably, the base oil is K-type perfluoropolyether or D type perfluoropolyether, the structural formula of the K-type perfluoropolyether
For：The wherein integer that m is 20~50；
The D type perfluoropolyether structures formula：CF3-CF2-CF2-O(CF2-CF2-CF2-O)nCF2CF3, wherein n is 20~50
Integer.
Preferably, the antioxidant anticorrosive agent is the benzotriazole of Rf modification, benzimidazole, benzopyrazoles, benzoxazoles
With one of benzothiazole or a variety of, structural formula is as follows：
The Rf is CxF2x-1-、C3F7O
(CF2CF2CF2O)yCF2CF2Or C3F7O{CF(CF3)CF2O}zCF(CF3)-one or more of, wherein x be 5~15 it is whole
Number, the integer that y is 5~15, the integer that z is 5~15.
Preferably, the antiwear additive is one of Perfluoropolyether amide alcohol or sulfur alcohol compound or a variety of, chemistry
Formula is RfCONH (CH2)pOH or RfCONH (CH2)pSH；The Rf is CxF2x-1-、C3F7O(CF2CF2CF2O)yCF2CF2Or
C3F7O{CF(CF3)CF2O}zCF(CF3One or more of)-, the integer that wherein p is 2~10, the integer that x is 5~15, y is
5~15 integer, the integer that z is 5~15.
Preferably, it is 90~98wt% that the base oil, which accounts for perfluoro polyether oil ratio, and the antioxidant anticorrosive agent accounts for
Perfluoro polyether oil ratio is 0.1~5wt%, and it is 0.1~5wt% that antiwear additive, which accounts for perfluoro polyether oil ratio,.
Beneficial effects of the present invention：
1. perfluoro polyether oil of the invention overcomes existing perfluoro polyether oil in high temperature and condition of boundary lubrication
Under the defect decomposed, can be applied to high temperature aero-turbine.At 300 DEG C, perfluoropolyether of the invention is used
Lubricating oil is continually fed into air 50h, carries out oxygen to aluminium LD-7, magnesium MB2, silver 1, titanium Tc-4, stainless steel GCr15 and M50 test piece
Change test, it is as a result corrosion-free；And lubricating oil viscosity change rate is only 3% or so after 50h；Illustrate perfluoropolyether of the invention
Lubricating oil has good oxidation stability, solves existing perfluoro polyether oil and is easy to decompose at high temperature and corrodes metal
Problem.
Used in 2. antioxidant anticorrosive agent and antiwear additive used in perfluoro polyether oil of the invention are dissolved in
In base oil, solve the problems, such as conventional additives insoluble in perfluoropolyether.
3. the experimental results showed that perfluoro polyether oil abrasion resistance of the invention is also improved.
4. preparation method of the invention is simple, it is particularly suitable for large-scale industrial production.
Specific embodiment
Embodiment 1-3 is the synthesis of antioxidant anticorrosive agent；Embodiment 4 is the synthesis of antiwear additive；Embodiment 5 is of the invention
The compounding of perfluoro polyether oil；Embodiment 6 and embodiment 7 are performance test.
Example 1：5- perfluoro hexyl benzotriazoleSynthesis：By 33.5g benzotriazole, 47g acetic acid
Sodium and 123g perfluoro-hexyl iodide (C6F13I it) is added sequentially in 1L stainless steel cauldron, with air in nitrogen displacement kettle, is warming up to
190 DEG C, stir 76h.It is cooled to room temperature, is filtered to remove sodium acetate, distilation obtains yellow viscous liquid 69g, as 5- perfluor
Hexyl benzotriazole, yield 56%.
Example 2：The synthesis of the benzopyrazoles of perfluoropolyether modification：Rf is C3F7O(CF2CF2CF2O)5CF2CF2-。
Under nitrogen protection, by 2.36g benzopyrazoles, the C of 270g3F7O(CF2CF2CF2O)5CF2CF2CFO, 100mL trifluoro
Trichloroethanes (F113) is added sequentially in 500mL there-necked flask, is stirred evenly, and 10mL triethylamine is then added, 6h is stirred at room temperature.
Washing removes triethylamine, dries, filters, and revolving removes solvent trifluorotrichloroethane (F113), and vacuum distillation obtains yellowish sticky
Liquid 240g, as
Example 3：The synthesis of the benzoxazoles of perfluoropolyether modification：Rf is C3F7O{CF(CF3)CF2O}3CF(CF3)-。
11g o-aminophenol, 50mL tetrahydrofuran are added sequentially to 250mL three-necked flask, mechanical stirring 10min is cold
But to 5 DEG C, 30mL n-BuLi (2M is dissolved in n-hexane) is slowly dropped into there-necked flask with constant pressure funnel under nitrogen protection
In, it maintains reacting liquid temperature at 5~10 DEG C, is added dropwise and continues to stir 30min.It is slow with constant pressure funnel under nitrogen protection
The C of 100g is added3F7O{CF(CF3)CF2O}3CF(CF3)-CFO, 1.5h is added dropwise, and continues to stir 2h, vacuum distillation removes four
Hydrogen furans, n-hexane, sand core funnel filtering, obtain 98g white liquid compound
Under nitrogen protection, the compound that will be obtained98g, which is added to, is connected with reflux condensate device
In 250mL three neck round bottom flask, 250 DEG C are heated to, stirs 20h, is cooled to room temperature, vacuum distillation obtains light yellow liquid 81g, i.e.,
For the benzoxazoles class additive of perfluoropolyether modificationYield 83%.
Example 4：Antiwear additive C3F7O{CF(CF3)CF2O}8CF(CF3)-CONH(CH2)2The synthesis of OH.
By the C of 100g3F7O{CF(CF3)CF2O}8CF(CF3)-COOCH3Add with the trifluorotrichloroethane (F113) of 100mL
Enter to dry 500mL three-necked flask, connect reflux unit, stirrer is added, temperature is set as 40 DEG C, etc. temperature reach setting
After temperature, ethanol amine is added by constant pressure funnel to three-necked flask in 30min, after being added dropwise, temperature is set as 65 DEG C,
This temperature is maintained to stir 5h.After reaction, reactant is moved in 500mL separatory funnel, successively uses ethyl acetate, dilute hydrochloric acid
It is dry with anhydrous magnesium sulfate with saturated salt solution washed product, remove moisture therein, filtering removal MgSO4 solid.Decompression is steamed
It evaporates to obtain the antiwear additive C of 80g3F7O{CF(CF3)CF2O}8CF(CF3)-CONH(CH2)2OH is colourless viscous liquid.
The compounding of the perfluoro polyether oil of the invention of example 5.
980g D type perfluoropolyether basis oily (number-average molecular weight about 6000) is added in 2L reaction kettle, mechanical stirring,
60 DEG C are slowly heated to, 10g antioxidant anticorrosive agent 5- perfluoro hexyl benzotriazole (embodiment 1 is made) is then added and 10g is anti-
Grinding agent C3F7O{CF(CF3)CF2O}8CF(CF3)-CONH(CH2)2OH (embodiment 4 is made), is warming up to 80 DEG C of stirring 1-2h, mixes
Filter residue is filtered to remove after uniformly at 80 DEG C and obtains the perfluoro polyether oil PFPE-1.PFPE-2 and PFPE- in table 1
3 base oil is D type perfluoropolyether, and additive is the PFPE lubricating oil of other different component ratios.
Table 1：Perfluoro polyether oil of the invention
| Lubricating oil number | Base oil content | Antioxidant anticorrosive agent content | Wear-resistant agent content |
| PFPE-1 | 98wt% | 1wt% (embodiment 1 is made) | 1wt% (embodiment 4 is made) |
| PFPE-2 | 95wt% | 3wt% (embodiment 2 is made) | 2wt% (embodiment 4 is made) |
| PFPE-3 | 90wt% | 4wt% (embodiment 3 is made) | 6wt% (embodiment 4 is made) |
Example 6：Perfluoro polyether oil (PFPE-1, PFPE-2 and PFPE-3 of embodiment 5) of the invention and existing complete
The corrosivity and oxidation stability of perfluoroalkyl polyether lubricating oil (the base oil of antioxidant anticorrosive agent and antiwear additive is not added for control sample)
It tests and compares.Referring to GJB499, test condition is：Lubricating oil is 165mL, and it is 165mL/min, temperature that air, which is passed through speed,
Degree is 300 DEG C, length of testing speech 50h, metal testing plate used be aluminium LD-7, steel GCr15 and steel M50 (internal diameter 6.3mm ± 0.1mm, outside
Diameter 19-20mm, thickness 2-3mm).Test result is as shown in table 2.
As can be seen from Table 2, corrosion of the existing perfluoro polyether oil (control sample) to aluminium LD-7, steel GCr15 and steel M50
Amount is respectively 0.09mg/cm2、1.26mg/cm2And 1.96mg/cm2；And PFPE-1, PFPE-2 and PFPE-3 are equal to three kinds of metals
It is corrosion-free；But the rate of change in viscosity and perfluoro polyether oil (control sample) of PFPE-1, PFPE-2 and PFPE-3 are almost the same.
Table 2：The corrosivity and oxidation stability test result of perfluoro polyether oil and control sample of the invention
Example 7：Perfluoro polyether oil of the invention and existing perfluoro polyether oil (control sample) lubricity under high temperature
It can test.
By in embodiment 5 PFPE-1, PFPE-2 and PFPE-3 and existing perfluoro polyether oil (control sample, i.e., not plus
Enter the base oil of antioxidant anticorrosive agent and antiwear additive) greasy property test is carried out on four-ball tester, condition is：Load
392N, 175 DEG C of temperature, revolving speed 1450rpm/min, time 30min.The results are shown in Table 3：Control sample is straight to average polishing scratch of trying
Diameter is 0.89mm；And PFPE-1, PFPE-2 and PFPE-3 to average grinding defect diameter of trying be respectively 0.60mm, 0.58mm and
0.55mm, the degree of wear tried are considerably lighter.Illustrate that perfluoro polyether oil abrasion resistance of the invention is also improved.
Table 3：The grinding defect diameter of perfluoro polyether oil and control sample of the invention
| Experimental condition load 392N, grinding defect diameter D (mm) | |
| Control sample | 0.89 |
| PFPE-1 | 0.60 |
| PFPE-2 | 0.58 |
| PFPE-3 | 0.55 |
Claims (10)
1. a kind of perfluoro polyether oil, which is characterized in that it is consisted of the following compositions：Base oil 90~98wt%, it is anti-oxidant
0.1~5wt% of corrosive agent, 0.1~5wt% of antiwear additive.
2. perfluoro polyether oil according to claim 1, which is characterized in that the base oil is K-type perfluoropolyether or D
The structural formula of type perfluoropolyether, the K-type perfluoropolyether is：Wherein m is 20
~50 integer；
The D type perfluoropolyether structures formula：CF3-CF2-CF2-O(CF2-CF2-CF2-O)nCF2CF3, wherein n be 20~50 it is whole
Number.
3. perfluoro polyether oil according to claim 1, which is characterized in that the antioxidant anticorrosive agent is Rf modification
One of benzotriazole, benzimidazole, benzopyrazoles, benzoxazoles and benzothiazole are a variety of, and structural formula is as follows： The Rf is CxF2x-1-、C3F7O(CF2CF2CF2O)yCF2CF2Or C3F7O{CF
(CF3)CF2O}zCF(CF3One or more of)-, the integer that wherein x is 5~15, the integer that y is 5~15, z is 5~15
Integer.
4. perfluoro polyether oil according to claim 1, which is characterized in that the antiwear additive is Perfluoropolyether amide alcohol
Or one of sulfur alcohol compound or a variety of, chemical formula are RfCONH (CH2)pOH or RfCONH (CH2)pSH, wherein p is 2
~10 integer；The Rf is CxF2x-1-、C3F7O(CF2CF2CF2O)yCF2CF2Or C3F7O{CF(CF3)CF2O}zCF(CF3)-
One or more of, the integer that wherein x is 5~15, the integer that y is 5~15, the integer that z is 5~15.
5. perfluoro polyether oil according to claim 1, which is characterized in that the viscosity 40 of the perfluoro polyether oil
DEG C when be 100~500mm2/ s, pour point are between -30 DEG C~-50 DEG C.
6. a kind of preparation method of perfluoro polyether oil according to claim 1, which is characterized in that including walking as follows
Suddenly：Base oil is heated to 60 DEG C, antioxidant anticorrosive agent and antiwear additive is added, is warming up to 80 DEG C of 1~2h of mixing, at this temperature
Filter residue is filtered to remove up to the perfluoro polyether oil.
7. preparation method according to claim 6, which is characterized in that the base oil is K-type perfluoropolyether or D type perfluor
The structural formula of polyethers, the K-type perfluoropolyether is：Wherein m is 20~50
Integer；
The D type perfluoropolyether structures formula：CF3-CF2-CF2-O(CF2-CF2-CF2-O)nCF2CF3, wherein n be 20~50 it is whole
Number.
8. preparation method according to claim 6, which is characterized in that the antioxidant anticorrosive agent is the benzo three of Rf modification
One of azoles, benzimidazole, benzopyrazoles, benzoxazoles and benzothiazole are a variety of, and structural formula is as follows： The Rf is CxF2x-1-、C3F7O(CF2CF2CF2O)yCF2CF2Or C3F7O{CF(CF3)CF2O}zCF
(CF3One or more of)-, the integer that wherein x is 5~15, the integer that y is 5~15, the integer that z is 5~15.
9. preparation method according to claim 6, which is characterized in that the antiwear additive is Perfluoropolyether amide alcohol or mercaptan
One of class compound is a variety of, and chemical formula is RfCONH (CH2)pOH or RfCONH (CH2)pSH, wherein p is 2~10
Integer；The Rf is CxF2x-1-、C3F7O(CF2CF2CF2O)yCF2CF2Or C3F7O{CF(CF3)CF2O}zCF(CF3)-in one
Kind is several, the integer that wherein x is 5~15, the integer that y is 5~15, the integer that z is 5~15.
10. preparation method according to claim 6, which is characterized in that the base oil accounts for perfluoro polyether oil ratio
For 90~98wt%, it is 0.1~5wt% that the antioxidant anticorrosive agent, which accounts for perfluoro polyether oil ratio, and it is poly- that antiwear additive accounts for perfluor
Ether lubricating oil ratio is 0.1~5wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810602648.4A CN108893176A (en) | 2018-06-12 | 2018-06-12 | A kind of perfluoro polyether oil and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810602648.4A CN108893176A (en) | 2018-06-12 | 2018-06-12 | A kind of perfluoro polyether oil and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108893176A true CN108893176A (en) | 2018-11-27 |
Family
ID=64344886
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810602648.4A Pending CN108893176A (en) | 2018-06-12 | 2018-06-12 | A kind of perfluoro polyether oil and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108893176A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110760361A (en) * | 2019-09-24 | 2020-02-07 | 中国石油化工股份有限公司 | Perfluoropolyether lubricating grease and preparation method thereof |
| CN110776974A (en) * | 2019-09-06 | 2020-02-11 | 中国石油化工股份有限公司 | High-temperature-resistant antirust perfluoropolyether lubricating oil and preparation method thereof |
| CN111876220A (en) * | 2020-08-04 | 2020-11-03 | 中国石油化工股份有限公司 | Chemical-medium-resistant fluorine-silicon lubricating grease and preparation method thereof |
| CN115466643A (en) * | 2022-09-15 | 2022-12-13 | 中国石油化工股份有限公司 | Low-temperature-resistant anti-wear fluorine lubricating oil |
| CN115521817A (en) * | 2022-10-18 | 2022-12-27 | 中国石油化工股份有限公司 | Lubricating oil antiwear additive, preparation method and application thereof |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1044951A (en) * | 1989-02-09 | 1990-08-29 | 奥西蒙特公司 | Have rust-preventing characteristic, be used as lubricating oil and the component of lubricating grease or the PFPE of additive |
| CN1052502A (en) * | 1989-12-12 | 1991-06-26 | 奥西蒙特公司 | Perfluoropolyether lubricant with antiwear properties |
| CN1914183A (en) * | 2004-01-30 | 2007-02-14 | 3M创新有限公司 | Perfluoropolyether benzotriazole derivatives and use thereof as coatings |
| US20080114177A1 (en) * | 2006-11-15 | 2008-05-15 | 3M Innovative Properties Company | Method for preparing fluorinated benzotriazole compounds |
| US20100267597A1 (en) * | 2009-04-21 | 2010-10-21 | Nok Kluber Co., Ltd. | Fluorine-based lubricant composition |
| CN102762706A (en) * | 2009-10-06 | 2012-10-31 | 索尔维特殊聚合物意大利有限公司 | Lubricant compositions for vacuum pumps |
| CN103031180A (en) * | 2011-09-30 | 2013-04-10 | 无锡市美城合成材料科技有限公司 | Grease |
| CN103476908A (en) * | 2010-12-23 | 2013-12-25 | 劳力士有限公司 | Composition for increasing the lipophobicity of a watch-making component |
| US20140000476A1 (en) * | 2010-12-23 | 2014-01-02 | Surfactis Technologies | Hydrophobic and lipophobic composition comprising compounds having a bisphosphonic and thiol group |
-
2018
- 2018-06-12 CN CN201810602648.4A patent/CN108893176A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1044951A (en) * | 1989-02-09 | 1990-08-29 | 奥西蒙特公司 | Have rust-preventing characteristic, be used as lubricating oil and the component of lubricating grease or the PFPE of additive |
| CN1052502A (en) * | 1989-12-12 | 1991-06-26 | 奥西蒙特公司 | Perfluoropolyether lubricant with antiwear properties |
| CN1914183A (en) * | 2004-01-30 | 2007-02-14 | 3M创新有限公司 | Perfluoropolyether benzotriazole derivatives and use thereof as coatings |
| US20080114177A1 (en) * | 2006-11-15 | 2008-05-15 | 3M Innovative Properties Company | Method for preparing fluorinated benzotriazole compounds |
| US20100267597A1 (en) * | 2009-04-21 | 2010-10-21 | Nok Kluber Co., Ltd. | Fluorine-based lubricant composition |
| CN102762706A (en) * | 2009-10-06 | 2012-10-31 | 索尔维特殊聚合物意大利有限公司 | Lubricant compositions for vacuum pumps |
| CN103476908A (en) * | 2010-12-23 | 2013-12-25 | 劳力士有限公司 | Composition for increasing the lipophobicity of a watch-making component |
| US20140000476A1 (en) * | 2010-12-23 | 2014-01-02 | Surfactis Technologies | Hydrophobic and lipophobic composition comprising compounds having a bisphosphonic and thiol group |
| CN103031180A (en) * | 2011-09-30 | 2013-04-10 | 无锡市美城合成材料科技有限公司 | Grease |
Non-Patent Citations (5)
| Title |
|---|
| BRADLEY A. SHOGRIN ET AL.: "Evaluation of Boundary-Enhancement Additives for Perfluoropolyethers", 《TRIBOLOGY TRANSACTIONS》 * |
| LOIS GSCHWENDER ET AL.: "Computational Chemistry of Soluble Additives for Perfluoropolyalkylether Liquid Lubricants", 《TRIBOLOGY TRANSACTIONS》 * |
| QUAN-FUWANG ET AL.: "A novel synthesis of 2-per(poly)fluoroalkyl-1H-benzimidazoles or 2-per(poly) fluoroalkyl benzothiazoles", 《JOURNAL OF FLUORINE CHEMISTRY》 * |
| 王大喜 等: "全氟聚醚润滑油添加剂抗氧抗腐蚀机理研究及分子设计─I.添加剂的作用机理和授受电子性质", 《中国科学（B辑）》 * |
| 王大喜: "N-取代全氟聚醚芳酰胺的分子结构特性", 《石油大学学报（自然科学版）》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110776974A (en) * | 2019-09-06 | 2020-02-11 | 中国石油化工股份有限公司 | High-temperature-resistant antirust perfluoropolyether lubricating oil and preparation method thereof |
| CN110760361A (en) * | 2019-09-24 | 2020-02-07 | 中国石油化工股份有限公司 | Perfluoropolyether lubricating grease and preparation method thereof |
| CN110760361B (en) * | 2019-09-24 | 2022-07-26 | 中国石油化工股份有限公司 | Perfluoropolyether lubricating grease and preparation method thereof |
| CN111876220A (en) * | 2020-08-04 | 2020-11-03 | 中国石油化工股份有限公司 | Chemical-medium-resistant fluorine-silicon lubricating grease and preparation method thereof |
| CN115466643A (en) * | 2022-09-15 | 2022-12-13 | 中国石油化工股份有限公司 | Low-temperature-resistant anti-wear fluorine lubricating oil |
| CN115521817A (en) * | 2022-10-18 | 2022-12-27 | 中国石油化工股份有限公司 | Lubricating oil antiwear additive, preparation method and application thereof |
| CN115521817B (en) * | 2022-10-18 | 2023-06-02 | 中国石油化工股份有限公司 | Lubricating oil antiwear additive and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108893176A (en) | A kind of perfluoro polyether oil and preparation method thereof | |
| Huang et al. | Investigation of the lubricity and antiwear behavior of guanidinium ionic liquids at high temperature | |
| EP1659165B1 (en) | Heterocyclic nitrogen containing (per)fluoropolyether additives for perfluoropolyether oils or greases | |
| CN103484224B (en) | A kind of gear oil composition and preparation method thereof | |
| JP2006144008A5 (en) | ||
| CN111876220B (en) | Chemical-medium-resistant fluorine-silicon lubricating grease and preparation method thereof | |
| CN106590906A (en) | Graphene oxide-containing water-based metal cutting fluid and preparation method thereof | |
| CN108130172A (en) | A kind of biodegradable environment-protective lubricant oil and preparation method thereof | |
| EP1712580A1 (en) | Additives for fluorinated oils | |
| McHugh et al. | Properties of a new class of polyaromatics for use as high-temperature lubricants and functional fluids | |
| US4438007A (en) | Perfluorinated aliphatic polyalkylether lubricant with an additive composed of an aromatic phosphine substituted with perfluoroalkylether groups | |
| El-Nagar et al. | Rheological and physical properties of ionic liquids with ammonium cations as synthetic lubricants | |
| CN107325857A (en) | One kind is used for high temperature low volatility Perfluoropolyether lubricating grease and preparation method | |
| CN110776974A (en) | High-temperature-resistant antirust perfluoropolyether lubricating oil and preparation method thereof | |
| Ding et al. | Tribological behavior of plant oil-based extreme pressure lubricant additive in water-ethylene glycol liquid | |
| CN107418651B (en) | Carboxylated triheptyl citrate calcium salt lubricating oil detergent and preparation method thereof | |
| CN109321341A (en) | A kind of water-sealed bearing waterproof lubricant grease and preparation method thereof | |
| CN111004662B (en) | Bio-based lubricating oil base oil and preparation method thereof | |
| CN107474912A (en) | A kind of high viscous finger, the Industrial gear oil composition of wide temperature range and its application | |
| US3306854A (en) | Corrosion inhibited poly(hexafluoropropylene oxide) oil compositions | |
| Singh et al. | Combined Effect of Phosphonium Ionic Liquid and Copper Oxide Nanopowder as Additives to the Bio-based Lubricant During Tribological Analysis | |
| CN109233941A (en) | A kind of ball shaped nano graphene lubricating oil and preparation method thereof | |
| CN113683506A (en) | Diester derivative type lubricating oil base oil and preparation method thereof | |
| CN1309126A (en) | S-(2H-thien-2-yl) methyl alkylxanthogenate | |
| Yao et al. | Insight into Hydrolytic Stability and Tribological Properties of BN Coordination Tung Oil-Based Lubricant Additive in Water. |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181127 |