CN108728207A - Rust-inhibiting additive and preparation method thereof and the application in perfluoro polyether oil - Google Patents
Rust-inhibiting additive and preparation method thereof and the application in perfluoro polyether oil Download PDFInfo
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- CN108728207A CN108728207A CN201810633977.5A CN201810633977A CN108728207A CN 108728207 A CN108728207 A CN 108728207A CN 201810633977 A CN201810633977 A CN 201810633977A CN 108728207 A CN108728207 A CN 108728207A
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- 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
- C10M149/00—Lubricating compositions characterised by the additive being a macromolecular compound containing nitrogen
- C10M149/12—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/002—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from unsaturated compounds
- C08G65/005—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from unsaturated compounds containing halogens
- C08G65/007—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from unsaturated compounds containing halogens containing fluorine
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- 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
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/041—Mixtures of base-materials and additives the additives being macromolecular compounds only
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2650/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G2650/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterized by the type of post-polymerisation functionalisation
- C08G2650/04—End-capping
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2650/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G2650/28—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type
- C08G2650/46—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type containing halogen
- C08G2650/48—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type containing halogen containing fluorine, e.g. perfluropolyethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2650/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G2650/28—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type
- C08G2650/50—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type containing nitrogen, e.g. polyetheramines or Jeffamines(r)
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- 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
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- 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
- C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2217/06—Macromolecular compounds obtained by functionalisation op polymers with a nitrogen containing compound
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Lubricants (AREA)
Abstract
The present invention provides a kind of rust-inhibiting additive and preparation method thereof and the application in perfluoro polyether oil, rust-inhibiting additive provided by the invention, has the following structure formula (I)：Rf in formula (I) isWherein m >=1, n >=1.The rust-inhibiting additive of the present invention is readily dissolved in perfluoro polyether oil, and can improve the rustless property of perfluoro polyether oil, and then the occurrence of can reduce equipment corrosion, extends service life of equipment.
Description
Technical field
The present invention relates to lube oil additive technical field, more particularly to a kind of rust-inhibiting additive and preparation method thereof, also
It is related to application of the rust-inhibiting additive in perfluoro polyether oil.
Background technology
Currently, perfluoro polyether oil is with its excellent low volatility, thermal stability, chemical stability, corrosion resistance characteristic
And property at high and low temperature and lubrication property, it is widely used in high temperature and harsh use environment.But make actual
With finding in the process, there is the case where corrosion in the metal parts using the relevant device of perfluoro polyether oil.Meanwhile to complete
Perfluoroalkyl polyether lubricating oil carries out in the test of liquid phase corrosion experiment, the test results of most perfluoro polyether oils be shown as middle rust or
It becomes rusty again, the poor serious use for limiting perfluoro polyether oil of rustless property.
In existing lubricating oil rust-inhibiting additive, it is largely primarily adapted for use in mineral lubricating oil and other synthetic oils.By
In the particularity of perfluoro polyether oil molecular structure, existing rust-inhibiting additive can not dissolve in perfluoro polyether oil,
Anti-rust action can not be played.
Invention content
In view of this, a kind of rust-inhibiting additive of present invention offer and its preparation method and application, antirust of the invention addition
Agent is readily dissolved in perfluoro polyether oil, and can improve the rustless property of perfluoro polyether oil, and then can reduce equipment
The occurrence of corrosion, extends service life of equipment.
The present invention is to reach its purpose, and the technical solution of use is as follows：
First aspect present invention provides a kind of rust-inhibiting additive, has the following structure formula (I)：
Rf in formula (I) isWherein m >=1, n >=
1。
The rust-inhibiting additive of the present invention, it is preferred that the molecular weight of the rust-inhibiting additive is in 2500g/mol-3800g/mol
Between.
Second aspect of the present invention provides a kind of preparation method of rust-inhibiting additive, includes the following steps,
(1) perfluoropolyether that end group is acyl fluorides is prepared
Tetrafluoroethene is added into reaction kettle, and is passed through oxygen into reaction kettle, temperature be -90 DEG C~-30 DEG C and
Poly-reaction is carried out under ultraviolet lighting, the end group for obtaining following structure formula (II) is the perfluoropolyether product of acyl fluorides：
Wherein, m >=1, n >=1；
(2) step (1) products therefrom is distilled, separation end group is the perfluoropolyether of acyl fluorides；
(3) preparation of rust-inhibiting additive
In a nitrogen atmosphere, using dimethylbenzene as azeotropic agent, by the perfluoropolyether and two that the end group obtained by step (2) is acyl fluorides
Ethylene triamine reacts 2-6h at 80-140 DEG C, is warming up to 160-230 DEG C of reaction 2-8h later, room is cooled in nitrogen atmosphere
Temperature removes removal xylene by vacuum distillation, obtains the rust-inhibiting additive.In this step, reaction is divided into two stages, 80-
140 DEG C of stages are reaction of the acyl fluorides with amino, and 160-230 DEG C of stage is the reaction that a closed loop forms imidazoline ring.
Preparation method of the present invention, it is preferred that in step (1), the charging rate of the tetrafluoroethene is 0.5-
The charging rate of 6kg/h, the oxygen are 50-4000L/h.
Preparation method of the present invention, it is preferred that in step (2), the process conditions of the distillation include：Pressure controls
For 5000 ± 500Pa, for fraction section temperature between 150 DEG C -200 DEG C, gained end group is the molecule of the perfluoropolyether fraction of acyl fluorides
Amount is 2500g/mol-3800g/mol.It is preferred that the intermediate product of this molecular weight ranges, final additive obtained has more
Moderate viscosity, it is easy to dissolve in application process.
Preparation method of the present invention, it is preferred that in step (3), the end group is the perfluoropolyether and diethyl of acyl fluorides
The molar ratio of alkene triamine is 1:1-1:3.
Third aspect present invention provides the purposes of rust-inhibiting additive described above, and the rust-inhibiting additive is applied to perfluor
In polyether oil, it is preferred that the dosage of the rust-inhibiting additive is in ‰ or more 3wt.
Technical solution provided by the invention has the advantages that：
The rust-inhibiting additive of the present invention, adds it in perfluoro polyether oil and is used as rust-inhibiting additive, according to
The requirement of GB/T 11143 is lubricated oily rustless property test, which can be dissolved completely in perfluoropolyether lubrication
Oil；Test result of the rust-inhibiting additive dosage in ‰ or more 3wt is rustless.
The rust-inhibiting additive of the present invention can be completely dissolved in perfluoro polyether oil, greatly improve perfluoropolyether lubrication
The rustless property of oil, and then the occurrence of reduction equipment corrosion, extend service life of equipment.
The rust-inhibiting additive preparation method of the present invention is simple and efficient, and reaction step is few, and the rust-inhibiting additive is without introducing
Phenyl ring, small toxicity are more environmentally friendly；Meanwhile the rust-inhibiting additive is with the i.e. changeable perfluoro polyether oil antirust of less additive amount
Performance, it is at low cost, it is more suitable for industrial production.
Description of the drawings
Fig. 1 is a kind of infrared spectrum of rust-inhibiting additive obtained in embodiment.
Fig. 2 be in a kind of embodiment end group obtained be acyl fluorides perfluoropolyether intermediate infrared spectrum.
Specific implementation mode
For a better understanding of the technical solution of the present invention, with reference to the embodiment content that the present invention is further explained,
But present disclosure is not limited only to following embodiment.Raw materials used in embodiment is marketable material, is repeated no more.
Embodiment 1
(1) end group is prepared by the perfluoropolyether of acyl fluorides
It is added tetrafluoroethene into reaction kettle with the charging rate of 1.5kg/h, while with the charging rate of 100L/h to anti-
Kettle is answered to be passed through oxygen, control reaction kettle internal temperature carries out poly-reaction at -40 DEG C under ultraviolet lighting, and it is acyl that end group, which is made,
The perfluoropolyether of fluorine, shown in products therefrom molecule such as formula (II).
(2) end group is the separation of the perfluoropolyether product of acyl fluorides
By step (1) products therefrom be added distillation still in, Distallation systm pressure control be 5000 ± 500Pa, heat temperature raising,
Fraction section of the collection temperature between 150 DEG C -200 DEG C is spare, and gained end group is that the perfluoropolyether fraction section molecular weight of acyl fluorides is
2500g/mol-3800g/mol；
The perfluoropolyether intermediate that gained end group is acyl fluorides is characterized using infrared spectrometer, as shown in Fig. 2, its
In：1984cm-1Place is the stretching vibration peak of-COF (acyl fluorides), 977cm-1Place is the stretching vibration peak of-C-O-C-, 809cm-1、
665cm-1Place is the stretching vibration peak of C-F keys.
(3) preparation of lubricating oil rust-inhibiting additive
It is continually fed into nitrogen into reactor, 400mL dimethylbenzene is added, mixing speed is set as 180rpm.By step (2)
The end group of gained is that reactor is added in the perfluoropolyether 3000g of acyl fluorides and 150g diethylenetriamines, is warming up to 90 DEG C of reaction 2.5h,
170 DEG C are continuously heating to, stops stirring and heating after reacting 4.5h, then the cooled to room temperature in nitrogen atmosphere passes through
Vacuum distillation removes removal xylene, and lubricating oil rust-inhibiting additive is made, shown in molecular structural formula such as formula (I), molecular weight and step (2)
Gained intermediate is not much different, between 2500g/mol-3800g/mol.
Gained lubricating oil rust-inhibiting additive is characterized using infrared spectrometer, sees Fig. 1, wherein：1706cm-1Place is C
=O carbonylic stretching vibrations peak, 1539cm-1Place is C=N double bond stretching vibration peaks, 1181cm-1Place is C-N singly-bound stretching vibrations
Peak, 808cm-1、745cm-1、716cm-1Place is the stretching vibration peak of C-F keys.
Lubricating oil rust-inhibiting additive obtained (or abbreviation antirust agent) is added in the perfluoro polyether oil of the different trades mark
Rustless property test is carried out according to GB/T 11143.
| Test oil product | Antirust agent additive amount (quality) | Test result |
| Fomblin Y25 | 3‰、6‰、10‰ | It is rustless |
| Fomblin Z15 | 3‰、6‰、10‰ | It is rustless |
| FM 120 | 3‰、6‰、10‰ | It is rustless |
Embodiment 2
(1) end group is prepared by the perfluoropolyether of acyl fluorides
It is added tetrafluoroethene into reaction kettle with the charging rate of 2.5kg/h, while with the charging rate of 600L/h to anti-
Kettle is answered to be passed through oxygen, control reaction kettle internal temperature carries out poly-reaction at -50 DEG C under ultraviolet lighting, and it is acyl that end group, which is made,
The perfluoropolyether of fluorine, shown in products therefrom molecule such as formula (II).
(2) end group is the separation of the perfluoropolyether product of acyl fluorides
By step (1) products therefrom be added distillation still in, Distallation systm pressure control be 5000 ± 500Pa, heat temperature raising,
Fraction section of the collection temperature between 150 DEG C -200 DEG C is spare, and gained end group is that the perfluoropolyether fraction section molecular weight of acyl fluorides is
2500g/mol-3800g/mol；
(3) preparation of lubricating oil rust-inhibiting additive
It is continually fed into nitrogen into reactor, 600mL dimethylbenzene is added, mixing speed is set as 200rpm.By step (2)
The end group of gained is that reactor is added in the perfluoropolyether 6000g of acyl fluorides and 240g diethylenetriamines, is warming up to 100 DEG C of reaction 4h,
200 DEG C are continuously heating to, stops stirring and heating after reacting 3.5h, then the cooled to room temperature in nitrogen atmosphere passes through
Vacuum distillation removes removal xylene, and lubricating oil rust-inhibiting additive is made, shown in molecular structural formula such as formula (I), molecular weight 2500g/
mol-3800g/mol。
Gained lube oil additive is characterized using infrared spectrometer, there are following absorption peaks for as a result display：
1706cm-1Place is C=O carbonylic stretching vibrations peak, 1539cm-1Place is C=N double bond stretching vibration peaks, 1181cm-1Place is that C-N is mono-
Key stretching vibration peak, 808cm-1、745cm-1、716cm-1Place is the stretching vibration peak of C-F keys.
Lubricating oil rust-inhibiting additive obtained (or abbreviation antirust agent) is added in the perfluoro polyether oil of the different trades mark
Rustless property test is carried out according to GB/T 11143.
| Test oil product | Antirust agent additive amount (quality) | Test result |
| Fomblin Y25 | 3‰、6‰、10‰ | It is rustless |
| Fomblin Z15 | 3‰、6‰、10‰ | It is rustless |
| FM 120 | 3‰、6‰、10‰ | It is rustless |
Embodiment 3
(1) end group is prepared by the perfluoropolyether of acyl fluorides
It is added tetrafluoroethene into reaction kettle with the charging rate of 4kg/h, while with the charging rate of 2000L/h to reaction
Kettle is passed through oxygen, and control reaction kettle internal temperature carries out poly-reaction at -80 DEG C under ultraviolet lighting, and it is acyl fluorides that end group, which is made,
Perfluoropolyether, shown in products therefrom molecule such as formula (II).
(2) end group is the separation of the perfluoropolyether product of acyl fluorides
By step (1) products therefrom be added distillation still in, Distallation systm pressure control be 5000 ± 500Pa, heat temperature raising,
Fraction section of the collection temperature between 150 DEG C -200 DEG C is spare, and gained end group is that the perfluoropolyether fraction section molecular weight of acyl fluorides is
2500g/mol-3800g/mol；
(3) preparation of lubricating oil rust-inhibiting additive
It is continually fed into nitrogen into reactor, 800mL dimethylbenzene is added, mixing speed is set as 180rpm.By step (2)
The end group of gained is that reactor is added in the perfluoropolyether 9000g of acyl fluorides and 320g diethylenetriamines, is warming up to 110 DEG C of reactions
4.5h is continuously heating to 210 DEG C, stops stirring and heating after reacting 6h, then the cooled to room temperature in nitrogen atmosphere is led to
It crosses decompression and dimethylbenzene is distilled off, lubricating oil rust-inhibiting additive is made, shown in molecular structural formula such as formula (I), molecular weight exists
Between 2500g/mol-3800g/mol.
Gained lube oil additive is characterized using infrared spectrometer, there are following absorption peaks for as a result display：
1706cm-1Place is C=O carbonylic stretching vibrations peak, 1539cm-1Place is C=N double bond stretching vibration peaks, 1181cm-1Place is that C-N is mono-
Key stretching vibration peak, 808cm-1、745cm-1、716cm-1Place is the stretching vibration peak of C-F keys.
Lubricating oil rust-inhibiting additive obtained (or abbreviation antirust agent) is added in the perfluoro polyether oil of the different trades mark
Rustless property test is carried out according to GB/T 11143.
| Test oil product | Antirust agent additive amount (quality) | Test result |
| Fomblin Y25 | 3‰、6‰、10‰ | It is rustless |
| Fomblin Z15 | 3‰、6‰、10‰ | It is rustless |
| 120 compressor oils of FM | 3‰、6‰、10‰ | It is rustless |
Embodiment 4
(1) end group is prepared by the perfluoropolyether of acyl fluorides
It is added tetrafluoroethene into reaction kettle with the charging rate of 5.2kg/h, while with the charging rate of 1600L/h to anti-
Kettle is answered to be passed through oxygen, control reaction kettle internal temperature carries out poly-reaction at -85 DEG C under ultraviolet lighting, and it is acyl that end group, which is made,
The perfluoropolyether of fluorine, shown in products therefrom molecule such as formula (II).
(2) end group is the separation of the perfluoropolyether product of acyl fluorides
By step (1) products therefrom be added distillation still in, Distallation systm pressure control be 5000 ± 500Pa, heat temperature raising,
Fraction section of the collection temperature between 150 DEG C -200 DEG C is spare, and gained end group is that the perfluoropolyether fraction section molecular weight of acyl fluorides is
2500g/mol-3800g/mol；
(3) preparation of lubricating oil rust-inhibiting additive
It is continually fed into nitrogen into reactor, 1000mL dimethylbenzene is added, mixing speed is set as 220rpm.By step
(2) end group obtained by is that reactor is added in the perfluoropolyether 10000g of acyl fluorides and 400g diethylenetriamines, is warming up to 105 DEG C of reactions
3.5h is continuously heating to 220 DEG C, stops stirring and heating after reacting 6h, then the cooled to room temperature in nitrogen atmosphere is led to
It crosses decompression and dimethylbenzene is distilled off, lubricating oil rust-inhibiting additive is made, shown in molecular structural formula such as formula (I), molecular weight exists
Between 2500g/mol-3800g/mol.
Gained lube oil additive is characterized using infrared spectrometer, the results showed that there are following absorption peaks：
1706cm-1Place is C=O carbonylic stretching vibrations peak, 1539cm-1Place is C=N double bond stretching vibration peaks, 1181cm-1Place is that C-N is mono-
Key stretching vibration peak, 808cm-1、745cm-1、716cm-1Place is the stretching vibration peak of C-F keys.
Lubricating oil rust-inhibiting additive obtained (or abbreviation antirust agent) is added in the perfluoro polyether oil of the different trades mark
Rustless property test is carried out according to GB/T 11143.
| Test oil product | Antirust agent additive amount | Test result |
| Fomblin Y25 | 3‰、6‰、10‰ | It is rustless |
| Fomblin Z15 | 3‰、6‰、10‰ | It is rustless |
| 120 compressor oils of FM | 3‰、6‰、10‰ | It is rustless |
In embodiment 1-4, obtained rust-inhibiting additive is easy to molten after the perfluoro polyether oil that the different trades mark are added
Solution.And moistened according to the requirement of GB/T 11143 as it can be seen that in the less amount of rust-inhibiting additive of the present invention of addition by experimental result
Lubricating oil rustless property is tested, and result is rustless.The rust-inhibiting additive of the present invention can greatly improve the anti-of perfluoro polyether oil
Rust performance, and then the occurrence of reduction equipment corrosion, extend service life of equipment；Simultaneously prepared by the rust-inhibiting additive of the present invention
Method is simple, and reaction step is few, and without introducing phenyl ring, small toxicity is suitble to industrial production and application.
It will be understood by those skilled in the art that under the introduction of this specification, the present invention can be made some modifications or
Adjustment.These modifications or adjustment should also be as within the scope of the claims in the present invention.
Claims (7)
1. a kind of rust-inhibiting additive, which is characterized in that have the following structure formula (I)：
Rf in formula (I) isWherein m >=1, n >=1.
2. rust-inhibiting additive according to claim 1, which is characterized in that the molecular weight of the rust-inhibiting additive is in 2500g/
Between mol-3800g/mol.
3. the preparation method of claim 1-2 any one of them rust-inhibiting additives, which is characterized in that include the following steps,
(1) perfluoropolyether that end group is acyl fluorides is prepared
Tetrafluoroethene is added into reaction kettle, and is passed through oxygen into reaction kettle, in temperature for -90 DEG C~-30 DEG C and ultraviolet
Poly-reaction is carried out under illumination, the end group for obtaining following structure formula (II) is the perfluoropolyether product of acyl fluorides：
Wherein, m >=1, n >=1；
(2) step (1) products therefrom is distilled, separation end group is the perfluoropolyether of acyl fluorides；
(3) preparation of rust-inhibiting additive
In a nitrogen atmosphere, using dimethylbenzene as azeotropic agent, by the perfluoropolyether and divinyl that the end group obtained by step (2) is acyl fluorides
Triamine reacts 2-6h at 80-140 DEG C, is warming up to 160-230 DEG C of reaction 2-8h later, is cooled to room temperature, leads in nitrogen atmosphere
It crosses decompression and dimethylbenzene is distilled off, obtain the rust-inhibiting additive.
4. preparation method according to claim 3, which is characterized in that in step (1), the charging rate of the tetrafluoroethene
Charging rate for 0.5-6kg/h, the oxygen is 50-4000L/h.
5. preparation method according to claim 3 or 4, which is characterized in that in step (2), the process conditions of the distillation
Including：Pressure control is 5000 ± 500Pa, and for fraction section temperature between 150 DEG C -200 DEG C, gained end group is that the perfluor of acyl fluorides is poly-
The molecular weight of ether fraction is 2500g/mol-3800g/mol.
6. according to claim 3-5 any one of them preparation methods, which is characterized in that in step (3), the end group is acyl fluorides
Perfluoropolyether and diethylenetriamine molar ratio be 1:1-1:3.
7. the purposes of claim 1-2 any one of them rust-inhibiting additives, which is characterized in that the rust-inhibiting additive is applied to
In perfluoro polyether oil, it is preferred that the dosage of the rust-inhibiting additive is in ‰ or more 3wt.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810633977.5A CN108728207A (en) | 2018-06-20 | 2018-06-20 | Rust-inhibiting additive and preparation method thereof and the application in perfluoro polyether oil |
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| CN201810633977.5A CN108728207A (en) | 2018-06-20 | 2018-06-20 | Rust-inhibiting additive and preparation method thereof and the application in perfluoro polyether oil |
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Cited By (2)
| 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 |
| 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 |
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| EP0976815A2 (en) * | 1998-07-31 | 2000-02-02 | The Lubrizol Corporation | Lubricating composition with improved bearing corrosion protection |
| CN102277577A (en) * | 2011-08-09 | 2011-12-14 | 陕西科技大学 | Fluorine-containing cationic imidazoline corrosion inhibitor and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
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