CN115710524B - Method for preparing extreme pressure antiwear perfluoropolyether grease and extreme pressure antiwear perfluoropolyether grease - Google Patents
Method for preparing extreme pressure antiwear perfluoropolyether grease and extreme pressure antiwear perfluoropolyether grease Download PDFInfo
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Abstract
A preparation method of extreme pressure anti-wear perfluoropolyether grease and extreme pressure anti-wear perfluoropolyether grease. The preparation method comprises the following steps: (1) Adding an extreme pressure antiwear additive into perfluoropolyether acyl fluoride, and carrying out surface modification under the action of fluorine gas to obtain a modified extreme pressure antiwear additive; (2) Adding the modified extreme pressure antiwear additive obtained in the step (1) into perfluoropolyether base oil, and uniformly mixing to obtain suspension; (3) Adding polytetrafluoroethylene thickener into the suspension obtained in the step (2), and uniformly mixing to obtain mixed colloid; (4) And (3) sequentially carrying out homogenization treatment and grinding treatment on the mixed colloid obtained in the step (3) to obtain the extreme pressure antiwear perfluoropolyether grease. The preparation method is simple and easy to operate, and the prepared extreme pressure antiwear perfluorinated polyether grease has good extreme pressure antiwear performance.
Description
Technical Field
The application belongs to the field of lubricating materials, and particularly relates to a preparation method of extreme pressure wear-resistant perfluoropolyether grease and extreme pressure wear-resistant perfluoropolyether grease.
Background
The perfluoro grease has long service cycle and excellent chemical stability, so that the range of using perfluoro grease is wider and wider, and the requirements on the performance of perfluoro grease are continuously improved. The perfluorinated lubricating grease can be contacted with various acid, alkali, salt, corrosive gas and strong oxidant mediums under the conditions of large temperature difference and long-period operation, and is required to have higher extreme pressure wear resistance.
CN 106108832A discloses a long-life high-temperature bearing grease and a preparation method thereof, but the stability of base oil is greatly different from that of perfluoropolyether. CN 109097163A discloses a long-life all-weather perfluoropolyether grease and a preparation method thereof, which uses perfluoropolyether as base oil and has better high-temperature and low-temperature resistance and rust resistance, but the extreme pressure wear resistance is not very ideal under special working conditions.
The prior perfluorinated lubricating grease can not meet the use requirements of some working conditions on the extreme pressure wear resistance.
Disclosure of Invention
The first aim of the application is to provide a preparation method of extreme pressure anti-wear perfluoropolyether grease, which is simple and easy to operate, and the prepared extreme pressure anti-wear perfluoropolyether grease has good extreme pressure anti-wear performance.
The second aim of the application is to provide the extreme pressure antiwear perfluoropolyether grease prepared by the preparation method, and the extreme pressure antiwear perfluoropolyether grease has good extreme pressure antiwear performance.
In order to achieve the first object of the present application, the following technical solutions are adopted:
a method for preparing extreme pressure antiwear perfluoropolyether grease, which comprises the following steps:
(1) Adding an extreme pressure antiwear additive into perfluoropolyether acyl fluoride, and carrying out surface modification under the action of fluorine gas to obtain a modified extreme pressure antiwear additive;
(2) Adding the modified extreme pressure antiwear additive obtained in the step (1) into perfluoropolyether base oil, and uniformly mixing to obtain suspension;
(3) Adding polytetrafluoroethylene thickener into the suspension obtained in the step (2), and uniformly mixing to obtain mixed colloid;
(4) And (3) sequentially carrying out homogenization treatment and grinding treatment on the mixed colloid obtained in the step (3) to obtain the extreme pressure antiwear perfluoropolyether grease.
The preparation method of the application is simple and easy to operate, and the prepared extreme pressure antiwear perfluoropolyether grease has excellent extreme pressure antiwear property.
Those skilled in the art understand that extreme pressure refers to the ability to bear loads without being forced out of the friction surface, resulting in a lack of lubrication of the friction surface; abrasion resistance refers to the ability of a grease to reduce friction against a friction surface and prevent wear.
In one embodiment, in step (1), the extreme pressure antiwear additive is molybdenum disulfide; preferably a mixture of molybdenum disulfide # 1 and molybdenum disulfide # 4; the preferred mass ratio of molybdenum disulfide # 1 to molybdenum disulfide # 4 is 1 (0.5-1.5), such as 1:0.6, 1:0.7, 1:0.8, 1:0.9, 1:1.0, 1:1.1, 1:1.2, 1:1.3, and 1:1.4.
In the present application, molybdenum disulfide # 1 is molybdenum disulfide having an average particle diameter d50=1.0 to 1.5 μm, and molybdenum disulfide # 4 is molybdenum disulfide having an average particle diameter d50=16.0 to 30.0 μm.
In one embodiment, in the step (1), the surface modification conditions are: under the condition of normal temperature and normal pressure, the modification is carried out for 3 to 5 hours, such as 3.25 hours, 3.5 hours, 3.75 hours, 4 hours, 4.25 hours, 4.5 hours and 4.75 hours; preferably, the mass ratio of extreme pressure antiwear additive to perfluoropolyether acyl fluoride is (0.5-1.5): 1, such as 0.6:1, 0.7:1, 0.8:1, 0.9:1, 1.0:1, 1.1:1, 1.2:1, 1.3:1, and 1.4:1.
Those skilled in the art understand that in the step (1), the extreme pressure antiwear additive is subjected to surface modification and then filtered, and the solid obtained by filtering is subjected to deacidification treatment, so that the modified extreme pressure antiwear additive is obtained.
Those skilled in the art understand that the extreme pressure antiwear additive has little change in quality before and after surface modification.
In one embodiment, the deacidification treatment is washing the solid obtained by filtration with an alkaline solution until the pH of the washing solution is 7; preferably, the alkaline solution is KOH/NaOH solution; preferably, the deacidification treatment further comprises continuing the washing with distilled water after the washing with the alkaline solution. Wherein the KOH/NaOH solution is a saturated/unsaturated solution of KOH/NaOH.
The person skilled in the art will understand that the aforementioned flushing liquid refers to the liquid that flows out after flushing the solids obtained by filtration.
In the application, the extreme pressure antiwear additive in the step (1) is modified to improve the affinity with the perfluoropolyether base oil, so that the combination property of the extreme pressure antiwear additive and the perfluoropolyether base oil is better.
In one embodiment, in step (2), the mixing comprises ultrasonic mixing, and the ultrasonic mixing temperature is 50-70 ℃, such as 55 ℃, 60 ℃ and 65 ℃, and the ultrasonic mixing time is 0.5-2 hours, such as 0.75 hours, 1 hour, 1.25 hours, 1.5 hours and 1.75 hours; preferably, the mixing further comprises stirring mixing, the stirring mixing is performed before the ultrasonic mixing, and the stirring mixing temperature is 50-70 ℃, such as 55 ℃, 60 ℃ and 65 ℃, and the stirring mixing time is 0.5-2h, such as 0.75h, 1h, 1.25h, 1.5h and 1.75h. Those skilled in the art will appreciate that ultrasonic mixing is performed in a water bath sonicator.
In one embodiment, in step (2), the perfluoropolyether base oil has the formulaWhere m, n are integers and m=1 to 100, such as 5, 10, 15, 20, 25, 30, 35, 40, 45, 50, 51, 55, 60, 65, 70, 75, 80, 85, 90 and 95, n=1 to 50, such as 5, 10, 15, 20, 25, 26, 30, 35, 40 and 45, r f1 And R is f2 Respectively selected from-CF 3 、—C 2 F 5 、—C 3 F 7 and-CF (CF) 3 )OCF 3 Any of the following; preferably the perfluoropolyether base oil has a molecular weight of 3000 to 10000g/mol, preferably 7000 to 9000g/mol, such as 7500g/mol, 8000g/mol and 8500g/mol.
Those skilled in the art understand that R f1 And R is f2 May be the same or different.
In an embodiment, in step (2), the mass ratio of the modified extreme pressure antiwear additive to the perfluoropolyether base oil is 1 (5-35), such as 1:5, 1:6.25, 1:7.5, 1:8.75, 1:10, 1:12.5, 1:15, 1:17.5, 1:20, 1:25, 1:30, and 1:35.
In one embodiment, in step (3), the mixing temperature is 50-70 ℃, such as 55 ℃, 60 ℃ and 65 ℃, and the mixing time is 0.5-2 hours, such as 0.75 hours, 1 hour, 1.25 hours, 1.5 hours and 1.75 hours; preferably, the mixing is stirring mixing.
In one embodiment, in step (3), the polytetrafluoroethylene thickener has an average particle size of 1 to 10 μm, such as 2 μm, 4 μm, 6 μm, and 8 μm; molecular weight of 1X (10 4 -10 9 ) g/mol, e.g. 1X 10 5 g/mol、1×10 6 g/mol、1×10 7 g/mol and 1X 10 8 g/mol。
In one embodiment, the mass ratio of the modified extreme pressure antiwear additive to the polytetrafluoroethylene thickener is 1 (2-20), such as 1:2, 1:2.5, 1:3, 1:3.75, 1:4, 1:5, 1:6, 1:7, 1:7.5, 1:8, 1:9, 1:10, 1:11, 1:12, 1:13, 1:14, 1:15, 1:16, 1:17, 1:18, 1:19, and 1:20.
In one embodiment, in the step (4), the homogenizing treatment is to perform homogenizing treatment on the mixed colloid obtained in the step (3) in a homogenizer to obtain a homogenized colloid; preferably, the homogenization treatment time is from 0.2 to 1h, such as 0.5h, to allow for more uniform mixing of the materials in the mixed colloid.
In one embodiment, in the step (4), the polishing process sequentially includes a first stage polishing process; the first-stage grinding treatment is to grind the homogenized colloid obtained by the homogenization treatment in a colloid dispersion mill to obtain a first grinding colloid, preferably grinding for 2-4 times, such as 3 times, so that the modified extreme pressure antiwear additive is better combined with the perfluoropolyether base oil, and the paste of the obtained extreme pressure antiwear perfluoropolyether grease is finer and has good lubricity; preferably, the grinding treatment further comprises a second stage grinding treatment in sequence, wherein the second stage grinding treatment is to grind the first grinding colloid obtained through the first stage grinding treatment in a grinder to obtain the extreme pressure antiwear perfluoropolyether grease, and the grinding time is preferably 1-3h, such as 1.5h, 2h and 2.5h.
It will be appreciated by those skilled in the art that the mill may be a conventional mill in the art, such as a three roll mill.
The person skilled in the art understands that the polytetrafluoroethylene thickener is agglomerated by nano-scale small particles, the inside of the polytetrafluoroethylene thickener is quite porous, and the perfluoropolyether base oil can be extruded into the pores in the polytetrafluoroethylene thickener through grinding extrusion, so that the perfluoropolyether base oil and the polytetrafluoroethylene thickener are better combined, and the paste of the obtained extreme-pressure antiwear perfluoropolyether grease is finer and has good lubricity.
The person skilled in the art understands that the extreme pressure antiwear perfluoropolyether grease obtained in the step (4) is subjected to vacuum degassing post-treatment and packaging in sequence, so as to obtain an extreme pressure antiwear perfluoropolyether grease product.
In order to achieve the second purpose, the application also provides extreme pressure wear-resistant perfluoropolyether grease prepared by the preparation method.
In one embodiment, the extreme pressure antiwear perfluoropolyether grease comprises the following substances in percentage by mass:
2-10wt% of modified extreme pressure antiwear additive, such as 4wt%, 5wt%, 6wt% and 8wt%;
50-70wt%, such as 55wt%, 60wt% and 65wt%, of the perfluoropolyether base oil;
the polytetrafluoroethylene thickener is 20-40wt%, such as 25wt%, 30wt% and 35wt%.
In one embodiment, the sum of the mass percentages of the modified extreme pressure antiwear additive, the perfluoropolyether base oil and the polytetrafluoroethylene thickener in the extreme pressure antiwear perfluoropolyether grease is 100wt%.
The application has the beneficial effects that:
the preparation method of the extreme pressure antiwear perfluoropolyether grease is simple and easy to operate, and the prepared extreme pressure antiwear perfluoropolyether grease has good extreme pressure antiwear performance, is not easy to extrude out of a friction surface when bearing load, can act on the friction surface for a long time, reduces friction and abrasion of the friction surface, and can be used in an environment of-40-260 ℃ to play a good lubricating protection role;
the extreme pressure antiwear perfluoropolyether grease prepared by the application has good extreme pressure antiwear performance, is not easy to be extruded out of a friction surface when bearing load, can act on the friction surface for a long time, reduces friction and abrasion of the friction surface, and can be used in an environment of-40-260 ℃ to play a good lubricating protection role.
Detailed Description
The technical scheme and effects of the present application are further described below with reference to specific embodiments. The following embodiments/examples are only for illustrating the contents of the present application, and the present application is not limited to the following embodiments or examples. Simple modifications of the application using the inventive concept are within the scope of the application as claimed.
The raw material sources are as follows:
molybdenum disulfide # 1, 99.5% pure, available from loma Shen Yumu, inc;
molybdenum disulfide # 4, 99.5% pure, available from loma Shen Yumu, inc;
perfluoro polyether acyl fluoride with molecular weight 4000-5000;
perfluoropolyether base oils of the formulaWherein m and n are integers, m=51-100, n=26-50, R f1 And R is f2 Respectively selected from-CF 3 、—C 2 F 5 、—C 3 F 7 and-CF (CF) 3 )OCF 3 Any of the following; the molecular weight is 7000-8000;
polytetrafluoroethylene thickeners available from nuo liter technology, inc.
Example 1 (S1)
The extreme pressure antiwear perfluoropolyether grease is prepared according to the following preparation method, and specifically comprises the following steps:
(1) Adding 20g of No. 1 molybdenum disulfide and 30g of No. 4 molybdenum disulfide into 100g of perfluoropolyether acyl fluoride, carrying out surface modification for 4 hours under the action of fluorine gas, filtering, flushing the solid obtained by filtering with a saturated solution of KOH until the pH value of flushing liquid is 7, and flushing with distilled water for 20s to obtain a modified extreme pressure antiwear additive;
(2) Adding the modified extreme pressure antiwear additive obtained in the step (1) into 700g of perfluoropolyether base oil, and ultrasonically mixing for 1h in a water bath ultrasonic device to obtain a suspension;
(3) Adding 300g of polytetrafluoroethylene thickener into the suspension obtained in the step (2), and stirring and mixing uniformly to obtain a mixed colloid;
(4) Homogenizing the mixed colloid obtained in the step (3) by using a homogenizer, grinding for 3 times by using a colloid dispersion mill, and grinding for 1h on a three-roller grinder to obtain the extreme pressure antiwear perfluoropolyether lubricating grease A1.
Example 2 (S2)
The extreme pressure antiwear perfluoropolyether grease is prepared according to the following preparation method, and specifically comprises the following steps:
(1) 50g of No. 1 molybdenum disulfide and 50g of No. 4 molybdenum disulfide are added into 100g of perfluoropolyether acyl fluoride, surface modification is carried out for 4 hours under the action of fluorine gas, then filtration is carried out, the solid obtained by filtration is washed by saturated solution of KOH until the pH value of washing liquid is 7, and then distilled water is used for washing for 10 seconds, thus obtaining the modified extreme pressure antiwear additive;
(2) Adding the modified extreme pressure antiwear additive obtained in the step (1) into 1500g of perfluoropolyether base oil, and ultrasonically mixing for 1.5h in a water bath ultrasonic device to obtain a suspension;
(3) Adding 500g of polytetrafluoroethylene thickener into the suspension obtained in the step (2), and stirring and mixing uniformly to obtain a mixed colloid;
(4) Homogenizing the mixed colloid obtained in the step (3) by using a homogenizer, grinding for 3 times by using a colloid dispersion mill, and grinding for 1.5 hours on a three-roller grinder to obtain the extreme pressure antiwear perfluoropolyether grease A2.
Example 3 (S3)
The extreme pressure antiwear perfluoropolyether grease is prepared according to the following preparation method, and specifically comprises the following steps:
(1) Adding 30g of No. 1 molybdenum disulfide and 40g of No. 4 molybdenum disulfide into 100g of perfluoropolyether acyl fluoride, carrying out surface modification for 3 hours under the action of fluorine gas, filtering, flushing the solid obtained by filtering with a saturated solution of KOH until the pH value of flushing liquid is 7, and flushing with distilled water for 10s to obtain a modified extreme pressure antiwear additive;
(2) Adding the modified extreme pressure antiwear additive obtained in the step (1) into 2200g of perfluoropolyether base oil, and ultrasonically mixing for 0.5h in a water bath ultrasonic device to obtain a suspension;
(3) Adding 700g of polytetrafluoroethylene thickener into the suspension obtained in the step (2), and stirring and mixing uniformly to obtain a mixed colloid;
(4) Homogenizing the mixed colloid obtained in the step (3) by using a homogenizer, grinding for 3 times by using a colloid dispersion mill, and grinding for 2 hours on a three-roller grinder to obtain the extreme pressure antiwear perfluoropolyether grease A3.
Example 4 (S4)
The extreme pressure antiwear perfluoropolyether grease is prepared according to the following preparation method, and specifically comprises the following steps:
(1) Adding 100g of No. 1 molybdenum disulfide and 50g of No. 4 molybdenum disulfide into 100g of perfluoropolyether acyl fluoride, carrying out surface modification for 5 hours under the action of fluorine gas, filtering, flushing the solid obtained by filtering with a saturated solution of KOH until the pH value of flushing liquid is 7, and flushing with distilled water for 10 seconds to obtain a modified extreme pressure antiwear additive;
(2) Adding the modified extreme pressure antiwear additive obtained in the step (1) into 2600g of perfluoropolyether base oil, and ultrasonically mixing for 1.5h in a water bath ultrasonic device to obtain a suspension;
(3) Adding 900g of polytetrafluoroethylene thickener into the suspension obtained in the step (2), and stirring and mixing uniformly to obtain a mixed colloid;
(4) Homogenizing the mixed colloid obtained in the step (3) by using a homogenizer, grinding for 3 times by using a colloid dispersion mill, and grinding for 2.5 hours on a three-roller grinder to obtain the extreme pressure antiwear perfluoropolyether grease A4.
Comparative example 1 (D1)
The preparation method of the perfluoropolyether grease comprises the following steps:
(1) 900g of polytetrafluoroethylene thickening agent is added into 2100g of perfluoropolyether base oil, and the mixture is stirred and mixed uniformly to obtain mixed colloid;
(2) Homogenizing the mixed colloid obtained in the step (1) by using a homogenizer, grinding for 3 times by using a colloid dispersion mill, and grinding for 1h on a three-roller grinder to obtain the perfluoropolyether lubricating grease B.
Testing and results
The extreme pressure antiwear perfluoropolyether greases A1 to A4 prepared in examples 1 to 4 (S1 to 4) and the perfluoropolyether grease B prepared in comparative example 1 (D1) were respectively subjected to the relevant performance tests, and the test results are shown in table 1.
The test results of the relative performance of the perfluoropolyether greases B obtained by the extreme pressure antiwear perfluoropolyether greases A1 to A4 and D1 obtained by tables 1S1 to 4
From examples 1-4 and comparative example 1, table 1 shows that:
in the application, whether the extreme pressure antiwear additive is added or not has little influence on the cone penetration, working temperature, pressure oil separation and evaporation degree of the obtained lubricating grease product; however, the addition of the extreme pressure antiwear additive can effectively improve the sintering load of the obtained extreme pressure antiwear perfluoropolyether grease product and greatly improve the PB value, thereby greatly improving the extreme pressure performance; in addition, the addition of the extreme pressure antiwear additive can also effectively reduce the friction coefficient of the obtained extreme pressure antiwear perfluoropolyether grease product and greatly reduce the abrasion spot diameter of the obtained grease product, thereby greatly improving the antiwear performance; this shows that the application can improve the extreme pressure antiwear property of the grease product without reducing the original property of the grease product by adding the corresponding extreme pressure antiwear additive.
Claims (16)
1. The preparation method of the extreme pressure wear-resistant perfluoropolyether grease is characterized by comprising the following steps of:
(1) Adding an extreme pressure antiwear additive into perfluoropolyether acyl fluoride, and carrying out surface modification under the action of fluorine gas to obtain a modified extreme pressure antiwear additive; wherein the extreme pressure antiwear additive is molybdenum disulfide; the surface modification conditions are as follows: modifying for 3-5h under normal temperature and normal pressure;
(2) Adding the modified extreme pressure antiwear additive obtained in the step (1) into perfluoropolyether base oil, and uniformly mixing to obtain suspension;
(3) Adding polytetrafluoroethylene thickener into the suspension obtained in the step (2), and uniformly mixing to obtain mixed colloid;
(4) And (3) sequentially carrying out homogenization treatment and grinding treatment on the mixed colloid obtained in the step (3) to obtain the extreme pressure antiwear perfluoropolyether grease.
2. The method according to claim 1, wherein in the step (1), the extreme pressure antiwear additive is a mixture of molybdenum disulfide # 1 and molybdenum disulfide # 4.
3. The method according to claim 2, wherein the mass ratio of molybdenum disulfide # 1 to molybdenum disulfide # 4 is 1 (0.5 to 1.5).
4. A method according to any one of claims 1 to 3, wherein in step (1), the mass ratio of the extreme pressure antiwear additive to the perfluoropolyether acyl fluoride is (0.5 to 1.5): 1.
5. The process of claim 1 wherein in step (2) the perfluoropolyether base oil has the formulaWherein m and n are integers, m=1-100, n=1-50, R f1 And R is f2 Respectively selected from-CF 3 、—C 2 F 5 、—C 3 F 7 and-CF (CF) 3 )OCF 3 Any of the above.
6. The process according to claim 5, wherein the perfluoropolyether base oil has a molecular weight of 3000 to 10000g/mol.
7. The process according to claim 6, wherein the perfluoropolyether base oil has a molecular weight of 7000 to 9000g/mol.
8. The process according to any one of claims 1 to 3 and 5 to 7, wherein in step (2), the mass ratio of the modified extreme pressure antiwear additive to the perfluoropolyether base oil is 1 (5 to 35).
9. The process according to claim 1, wherein in the step (3), the polytetrafluoroethylene thickener has an average particle diameter of 1 to 10. Mu.m, and a molecular weight of 1X (10 4 -10 9 )g/mol。
10. The method according to any one of claims 1 to 3, 5 to 7 and 9, wherein the mass ratio of the modified extreme pressure antiwear additive to the polytetrafluoroethylene thickener is 1 (2 to 20).
11. The method according to claim 1, wherein in the step (3), the mixing temperature is 50 to 70℃and the mixing time is 0.5 to 2 hours.
12. The method according to claim 11, wherein the mixing in the step (3) is stirring mixing.
13. The method according to any one of claims 1 to 3, 5 to 7, 9 and 11 to 12, wherein in the step (2), the mixing comprises ultrasonic mixing, and the ultrasonic mixing temperature is 50 to 70 ℃ and the ultrasonic mixing time is 0.5 to 2 hours.
14. The method according to claim 13, wherein in the step (2), the mixing further comprises stirring and mixing, the stirring and mixing is performed before the ultrasonic mixing, and the stirring and mixing temperature is 50-70 ℃ and the stirring and mixing time is 0.5-2h.
15. An extreme pressure antiwear perfluoropolyether grease prepared by the method of any one of claims 1-14.
16. The extreme pressure antiwear perfluoropolyether grease of claim 15, wherein the extreme pressure antiwear perfluoropolyether grease comprises the following substances in percentage by mass:
2-10wt% of modified extreme pressure antiwear additive
50-70wt% of perfluoropolyether base oil
20-40wt% of polytetrafluoroethylene thickener.
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| CN117660078A (en) * | 2023-11-24 | 2024-03-08 | 广州友乐润滑材料有限公司 | Composite lubricating grease and preparation method thereof |
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