CN104611101A - Perfluoropolyether lubricating grease and preparation method thereof - Google Patents
Perfluoropolyether lubricating grease and preparation method thereof Download PDFInfo
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- CN104611101A CN104611101A CN201410728148.7A CN201410728148A CN104611101A CN 104611101 A CN104611101 A CN 104611101A CN 201410728148 A CN201410728148 A CN 201410728148A CN 104611101 A CN104611101 A CN 104611101A
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Abstract
The invention relates to a perfluoropolyether lubricating grease and a preparation method thereof. The lubricating grease is composed of the following components, by weight: 60-80% of fluorine-containing base oil, 10-30% of a thickening agent, 0.3-1.0% of an antioxidant, 2-6% of a rust inhibitor, and 3-8% of an anti-wear extreme pressure agent. The invention also discloses a preparation method of the lubricating grease. With the perfluoropolyether lubricating grease, friction during a gear operation process can be reduced; gear corrosion degree can be reduced; rolling bearing high-temperature performance can be improved; rolling bearing low-temperature operation noise can be reduced; and environment pollution can be reduced.
Description
Technical field
The present invention relates to technical field of lubricant, be specifically related to a kind of Perfluoropolyether lubricating grease and preparation method thereof.
Technical background
In recent years, grow with each passing day along with to production automotive needs that is small and exquisite, light and low noise.Therefore electric component that is small and exquisite, light and low noise will be produced accordingly.Because the life-span being sealed in the lubricating grease in rolling bearing is shorter than the life-span of the rolling bearing of tired running, and the life-span of rolling bearing depends on the life-span of lubricating grease, and therefore, a kind of good lubricating grease directly decides the time limit of service of automobile and other equipment.It is wide that PFPE possesses use temperature scope, and there is low pour point, low volatility, biologically inert compatible/incombustible with plastics, rubber and metal and be only dissolved in the medium feature of organic solvent in perfluor organic solvent, excellent stability is at high temperature possessed as the tetrafluoroethylene (PTFE) of viscosifying agent and derivative thereof, and the advantage such as chemical resistant properties is good.The Perfluoropolyether lubricating grease that both are prepared into can meet the rolling bearing of high vacuum, high temperature and low temperature use and the application requiring of gear.
Perfluoropolyether lubricating grease is by PFPE basis oil (PFPE) multiviscosisty of fluorocarbon resin powder and high chemical stability, and adds Special Anti corrosion additive compound and become white mass.These parts being exclusively used in the bearing in high temperature, high capacity, corrosive chemical environments containing fluorenone and requiring lifelong lubrication, have splendid unreactiveness, weather resistance and low volatility.Be applicable to the components and parts in high temperature and low-temperature working.
Chinese patent application CN103710080A discloses a kind of preparation method for high/low temperature vacuum system and the lubrication of high/low temperature vacuum valve and the high-low temperature resistant siloxanes vacuum grease composition of sealing, this valve uses SiO 2 powder to be viscosifying agent, but silica product causes it aobvious acid due to the reason of processing process, if not to it through pyroprocessing, be difficult to obtain neutral SiO 2 powder, also just cause siloxane grease in the long-time shortcoming storing and exist in use procedure sealing property and reduce.US Patent No. 20040198612 discloses a kind of preparation method of double composition grease, this mixed grease comprises containing fluorenone with containing urea grease, the price of the Perfluoropolyether lubricating grease being used alone oil based on PFPE can be reduced in degree definitely, but there is the shortcoming of complicated process of preparation.Patent CN 103031180B prepares a kind of containing the Perfluoropolyether lubricating grease composition of hexagonal boron nitride as thickening material, avoid the use of tetrafluoroethylene, and do not use any additive, but the long life test of high temperature is not carried out to it, the long stability of its high temperature cannot be determined.
Summary of the invention
In order to overcome defect and the deficiency of prior art, the object of the present invention is to provide a kind of lubricating grease formula that can use under high temperature and low temperature and vacuum environment, the lubricating grease that this formula configures also possesses good oxidation-resistance, erosion resistance and abrasion resistant extreme-pressure simultaneously.
Technical scheme of the present invention provides a kind of Perfluoropolyether lubricating grease, it is characterized in that, the described weight percent containing each component of fluorenone is:
Described fluorine-containing base oil is formula I:
Wherein 30≤n≤90;
Described viscosifying agent is fluorocarbon resin powder, and described fluorocarbon resin powder is selected from the one in tetrafluoroethylene, tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer or tetrafluoroethylene propylene copolymer;
Described antioxidant is selected from the mixture of liquid octyl group butyl pentanoic oxidation inhibitor or Butylated Diphenylamine and octylated diphenylamine;
Described rust-preventive agent is selected from sulfonate or cyclamate;
Described extreme pressure additive is sulfide isobutene.
According to the lubricating grease that technique scheme provides, PFPE molecular weight is between 5000-15000, and kinematic viscosity when 40 DEG C is 50-900cSt.
According to the lubricating grease that technique scheme provides, grinding is carried out in three-roller.
Another technical scheme of the present invention provides the method preparing lubricating grease, comprise the following steps: thickening material is added in the reactor that 80-110 DEG C of base oil is housed, be warming up to 130 DEG C, 80 DEG C are cooled to after stirring 2-5h, add antioxidant, rust-preventive agent and additive, be cooled to room temperature after mixing, namely grinding, de-vacuum obtain product.
Unless explicitly stated otherwise in contrast, otherwise all scopes that the present invention quotes comprise end value.Such as, " wherein n is the integer of 30-90 ", represents that the polymerization degree in PFPE is 30≤n≤90.
The definition "or" that the present invention uses represents alternatives, if properly, they can be combined, and that is, term "or" comprises each listed independent alternatives and their combination.Such as, " described rust-preventive agent is selected from sulfonate or cyclamate " represents that rust-preventive agent can be the one among sulfonate and cyclamate, also can be its more than one combination.
The water used in embodiments of the present invention is deionized water.
Beneficial effect of the present invention is:
1) Perfluoropolyether lubricating grease provided by the invention, is mainly used in gear and rolling bearing, possesses the advantage can stablizing use at high temperature and low temperature and vacuum environment.This Perfluoropolyether lubricating grease is applied in the work-ing life that can extend bearing in rolling bearing, and the bearing under high temperature operation does not produce fatigue effect; Be applied to the generation that can suppress noise in the bearing of low-temperature working, there is the features such as lower frictional coefficient;
2) Perfluoropolyether lubricating grease provided by the invention, there is excellent erosion resistance, oxidation-resistance, gear and rolling bearing effectively can be prevented to be corroded, there is good abrasion resistant extreme-pressure simultaneously, decrease the friction in gear and rolling bearing operational process;
3) preparation technology of the present invention is simple, and cost is low, is conducive to suitability for industrialized production.
Embodiment
The following stated be the preferred embodiment of the present invention, what the present invention protected is not limited to following preferred implementation.It should be pointed out that on the basis of conceiving in these innovation and creation for a person skilled in the art, the some distortion made and improvement, all belong to protection scope of the present invention.Raw material used in embodiment all can be obtained by commercial sources.
Sulfide isobutene (Anglamol 23) is purchased from Lubrizol Corp.; Liquid octyl group butyl pentanoic oxidation inhibitor
with the mixture of Butylated Diphenylamine and octylated diphenylamine
all purchased from Crompton company, fluorine-containing base oil is available from DuPont
perfluoro polyether oil (K type PFPE).
Embodiment 1
First in stirred autoclave, add polymerization degree K type PFPE between 30-90 of 70%, after being warming up to 100 DEG C, add the thickening material tetrafluoroethylene of 20%, be warming up to 130 DEG C and stir 3h, after being cooled to 80 DEG C, add 0.5%
antioxidant, the rust-preventive agent sulfonate of 3.5%, the wear preventive additive Anglamol 23 of 6%, mixes rear taking-up, is cooled to room temperature, joins in three-roller and grinds three times, obtain product after Fruit storage.Product performance characterize as shown in table 1.
To extreme pressure power, pour point, the frictional coefficient of obtained Perfluoropolyether lubricating grease composition, low temperature whether produces noise and high-temperature stability is tested, and testing method is as follows:
Extreme pressure power:
Use four ball testing method, according to the extreme pressure of SH/T0202-92 (lubricating grease extreme pressure property assay method) measuring lubricating grease.
Frictional coefficient:
Perfluoropolyether lubricating grease composition is coated on SPCC-SB steel plate, thickness is about 0.1mm, place 1/2 inch steel ball, load heavy 1.96N, sliding velocity 30cpm, sliding distance 40mm, under the probe temperature of 25 DEG C, slide 1000 this carry out come and go test, pass through load cell, export frictional force from recording instrumnet, calculate the frictional coefficient after this test of slip circulation 1000.
Pour point:
According to the pour point of ASTM D97-96a measuring lubricating grease.After samples pre-heated, cool in specific temperature range, and be its mobility of interval measurement with every 3 DEG C.The minimum temperature that sample can flow, is the pour point of this sample.
Noise:
By grease sealing in the 6203LLHA rolling bearing that sherwood oil is cleaned, rolling bearing is inserted in the low temperature bath of-60 DEG C, when the temperature of rolling bearing itself reaches-60 DEG C, is taken out, as under room temperature condition.Rolling bearing, under the radial load of 2700rpm, 127N, observes whether generate noise.
High-temperature stability:
By grease sealing in the 6204ZZ rolling bearing that sherwood oil is cleaned, according to the high-temperature stability of D3336-1997 measuring lubricating grease.
Embodiment 2
First in stirred autoclave, add the polymerization degree of 70% between the K type PFPE of 30-90, after being warming up to 100 DEG C, add the thickening material tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer of 20%, be warming up to 130 DEG C and stir 4h, after being cooled to 80 DEG C, add 0.5%
antioxidant, the rust-preventive agent sulfonate of 2.5%, the wear preventive additive Anglamol 23 of 4%, takes out after stirring, is cooled to room temperature, joins in three-roller and grinds three times, obtain product after Fruit storage.Testing method is with embodiment 1, and product performance characterize in table 1.
Embodiment 3
First in stirred autoclave, add the polymerization degree of 70% between the K type PFPE of 30-90, after being warming up to 110 DEG C, add the thickening material tetrafluoroethylene of 24%, be warming up to 130 DEG C and stir 5h, after being cooled to 80 DEG C, add 0.3%
antioxidant, the rust-preventive agent cyclamate of 2.7%, the wear preventive additive Anglamol 23 of 4%, take out after stirring, be cooled to room temperature, join in three-roller and grind three times, obtain product after Fruit storage, testing method is with embodiment 1, and product performance characterize in table 1.
Embodiment 4
First in stirred autoclave, add the polymerization degree of 80% between the K type PFPE of 30-90, after being warming up to 80 DEG C, add the thickening material fluorinated ethylene propylene copolymer of 13%, be warming up to 130 DEG C and stir 2h, after being cooled to 80 DEG C, add 0.5%
antioxidant, the rust-preventive agent cyclamate of 2.5%, the wear preventive additive Anglamol 23 of 4%, take out after stirring, be cooled to room temperature, add in three-roller and grind three times, obtain product after Fruit storage, testing method is with embodiment 1, and product performance characterize in table 1.
Embodiment 5
First the polymerization degree adding 60% in stirred autoclave between the K type PFPE of 30-90, base oil be warming up to 100 DEG C, then add the thickening material tetrafluoroethylene of 30%, be warming up to 130 DEG C and stir 4h, after being cooled to 80 DEG C, add 0.8%
antioxidant, the rust-preventive agent cyclamate of 4.2%, the wear preventive additive Anglamol 23 of 5%, take out after stirring, be cooled to room temperature, add in three-roller and grind three times, obtain product after Fruit storage, testing method is embodiment 1 simultaneously, and product performance characterize in table 1.
The Performance Detection of the different embodiment of table 1
| Performance index | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Extreme pressure power (N) | 9260 | 8620 | 8060 | 8620 | 8640 |
| Pour point (DEG C) | ≥250 | ≥250 | ≥250 | ≥250 | ≥250 |
| Frictional coefficient | 0.12 | 0.14 | 0.15 | 0.14 | 0.13 |
| Whether low temperature produces noise | No | No | No | No | No |
| High-temperature stability (180 DEG C, h) | ≥4000 | ≥4000 | ≥4000 | ≥4000 | ≥4000 |
Claims (4)
1. a Perfluoropolyether lubricating grease, is characterized in that, the weight percent of each component of described Perfluoropolyether lubricating grease is:
Described base oil is type I compound:
Wherein 30≤n≤90;
Described viscosifying agent is fluorocarbon resin powder, and described fluorocarbon resin powder is selected from the one in tetrafluoroethylene, tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer or tetrafluoroethylene propylene copolymer;
Described antioxidant is selected from the mixture of liquid octyl group butyl pentanoic oxidation inhibitor or Butylated Diphenylamine and octylated diphenylamine;
Described rust-preventive agent is selected from sulfonate or cyclamate;
Described extreme pressure additive is sulfide isobutene.
2. Perfluoropolyether lubricating grease according to claim 1, is characterized in that, described PFPE molecular weight is between 5000-15000, and kinematic viscosity when 40 DEG C is 50-900cSt.
3. Perfluoropolyether lubricating grease according to claim 1, is characterized in that, described fluorocarbon resin powder is selected from tetrafluoroethylene, tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer or tetrafluoroethylene propylene copolymer.
4. the preparation method of Perfluoropolyether lubricating grease described in a claim 1-3, it is characterized in that, comprise the following steps: thickening material is added in the reactor that 80-110 DEG C of base oil is housed, be warming up to 130 DEG C, 80 DEG C are cooled to after stirring 2-5h, add antioxidant, rust-preventive agent and additive, be cooled to room temperature after mixing, namely grinding, de-vacuum obtain product.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105018195A (en) * | 2015-06-23 | 2015-11-04 | 东莞市佳丹润滑油有限公司 | Special lubricant for plastic part assembly, and preparation method thereof |
| CN105670757A (en) * | 2016-03-14 | 2016-06-15 | 衢州学院 | Fluorine polymer polymeric wax modified long-chain alkyl silicone oil lubricating grease composition and preparation method thereof |
| CN106589993A (en) * | 2016-12-19 | 2017-04-26 | 安徽世界村新材料有限公司 | High temperature-resistant and highly-stable waste rubber powder modified waterproof coil asphalt material and preparation method thereof |
| CN107325857A (en) * | 2017-08-26 | 2017-11-07 | 东莞市欧迪斯润滑剂科技有限公司 | One kind is used for high temperature low volatility Perfluoropolyether lubricating grease and preparation method |
| CN107338084A (en) * | 2017-05-30 | 2017-11-10 | 刘秀梅 | A kind of high cold-resistant lubricating grease |
| CN107629852A (en) * | 2017-10-20 | 2018-01-26 | 安徽中天石化股份有限公司 | A kind of wear-resisting lubricating grease and preparation method thereof |
| CN107653037A (en) * | 2017-09-26 | 2018-02-02 | 中国石油化工股份有限公司 | A kind of Perfluoropolyether lubricant and preparation method thereof |
| CN107723066A (en) * | 2017-09-26 | 2018-02-23 | 中国石油化工股份有限公司 | A kind of PFPE type rubber seal fat and preparation method thereof |
| CN107760409A (en) * | 2017-12-06 | 2018-03-06 | 东莞市欧迪斯润滑剂科技有限公司 | A kind of extremely low volatility fluorine element lubricating grease and preparation method |
| CN108264956A (en) * | 2016-12-30 | 2018-07-10 | 东莞东阳光科研发有限公司 | A kind of high temperature resistant Perfluoropolyether lubricating grease |
| CN108715768A (en) * | 2018-06-27 | 2018-10-30 | 中国石油化工股份有限公司 | A kind of long-life high temperature bearing Perfluoropolyether lubricating grease and its preparation method and application |
| CN109097163A (en) * | 2018-06-29 | 2018-12-28 | 中国石油化工股份有限公司 | A kind of long-life round-the-clock Perfluoropolyether lubricating grease and its preparation method and application |
| CN110791357A (en) * | 2019-08-16 | 2020-02-14 | 中国石油化工股份有限公司 | Anti-radiation lubricating grease and preparation method thereof |
| CN111100724A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Perfluoropolyether lubricating grease and preparation method thereof |
| CN111100731A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Lubricating grease and preparation method thereof |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105018195A (en) * | 2015-06-23 | 2015-11-04 | 东莞市佳丹润滑油有限公司 | Special lubricant for plastic part assembly, and preparation method thereof |
| CN105670757B (en) * | 2016-03-14 | 2018-11-16 | 衢州学院 | Modified long-chain alkyl-silicone oil lubricant composition of a kind of fluoropolymer micro mist wax and preparation method thereof |
| CN105670757A (en) * | 2016-03-14 | 2016-06-15 | 衢州学院 | Fluorine polymer polymeric wax modified long-chain alkyl silicone oil lubricating grease composition and preparation method thereof |
| CN106589993A (en) * | 2016-12-19 | 2017-04-26 | 安徽世界村新材料有限公司 | High temperature-resistant and highly-stable waste rubber powder modified waterproof coil asphalt material and preparation method thereof |
| CN108264956A (en) * | 2016-12-30 | 2018-07-10 | 东莞东阳光科研发有限公司 | A kind of high temperature resistant Perfluoropolyether lubricating grease |
| CN108264956B (en) * | 2016-12-30 | 2022-02-15 | 东莞东阳光科研发有限公司 | High-temperature-resistant perfluoropolyether lubricating grease |
| CN107338084A (en) * | 2017-05-30 | 2017-11-10 | 刘秀梅 | A kind of high cold-resistant lubricating grease |
| CN107325857A (en) * | 2017-08-26 | 2017-11-07 | 东莞市欧迪斯润滑剂科技有限公司 | One kind is used for high temperature low volatility Perfluoropolyether lubricating grease and preparation method |
| CN107653037A (en) * | 2017-09-26 | 2018-02-02 | 中国石油化工股份有限公司 | A kind of Perfluoropolyether lubricant and preparation method thereof |
| CN107723066A (en) * | 2017-09-26 | 2018-02-23 | 中国石油化工股份有限公司 | A kind of PFPE type rubber seal fat and preparation method thereof |
| CN107629852A (en) * | 2017-10-20 | 2018-01-26 | 安徽中天石化股份有限公司 | A kind of wear-resisting lubricating grease and preparation method thereof |
| CN107760409A (en) * | 2017-12-06 | 2018-03-06 | 东莞市欧迪斯润滑剂科技有限公司 | A kind of extremely low volatility fluorine element lubricating grease and preparation method |
| CN108715768A (en) * | 2018-06-27 | 2018-10-30 | 中国石油化工股份有限公司 | A kind of long-life high temperature bearing Perfluoropolyether lubricating grease and its preparation method and application |
| CN109097163A (en) * | 2018-06-29 | 2018-12-28 | 中国石油化工股份有限公司 | A kind of long-life round-the-clock Perfluoropolyether lubricating grease and its preparation method and application |
| CN111100724A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Perfluoropolyether lubricating grease and preparation method thereof |
| CN111100731A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Lubricating grease and preparation method thereof |
| CN111100724B (en) * | 2018-10-25 | 2022-07-15 | 中国石油化工股份有限公司 | Perfluoropolyether lubricating grease and preparation method thereof |
| CN110791357A (en) * | 2019-08-16 | 2020-02-14 | 中国石油化工股份有限公司 | Anti-radiation lubricating grease and preparation method thereof |
| CN110791357B (en) * | 2019-08-16 | 2022-07-26 | 中国石油化工股份有限公司 | Anti-radiation lubricating grease and preparation method thereof |
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