CN101696366A - Method for preparing lubricating grease with excellent anti-wear and wear-resistant performance - Google Patents
Method for preparing lubricating grease with excellent anti-wear and wear-resistant performance Download PDFInfo
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- CN101696366A CN101696366A CN200910236610A CN200910236610A CN101696366A CN 101696366 A CN101696366 A CN 101696366A CN 200910236610 A CN200910236610 A CN 200910236610A CN 200910236610 A CN200910236610 A CN 200910236610A CN 101696366 A CN101696366 A CN 101696366A
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Abstract
The invention discloses a method for preparing polyurea lubricating grease with high PB value. By changing an addition process of an additive, the additive is used as a part of base oil to undergo a thickening reaction so as to double the wear-resistant extreme pressure effect of the additive, reduce the proportion of the anti-wear and wear-resistant additive and improve economic efficiency, and the preparation method is favorable for environmental protection. An ureido lubricating grease composite consists of the base oil, a thickening agent and the additive; and the base oil is a mixture of various kinds of mineral base oil, synthetic oil, tackifier and anti-wear and wear-resistant additives. The polyurea lubricating grease prepared by the method has the excellent anti-wear and wear-resistant performance, has the maximum nonseizure load PB of over 135 kilograms, has the characteristics of high drop point, low noise and strong adhesivity, can be used for machinery lubrication under the severe operating conditions, such as high temperature, overloading, moist, harmful media and the like and can be used as bearing lubricating grease for bearings operating at a high speed and a superspeed.
Description
Technical field
The invention belongs to the preparation of greases method.
Background technology
The modern machinery and equipment correlation parameter improves day by day, and working load is more and more heavier, and it is harsh that applying working condition is tending towards, and these are all having a strong impact on the wear pattern and the work-ing life of mechanical component.The lubricated operating mode of this harshness, especially outstanding for the high-speed bearing industry, because high-speed bearing is very sensitive to wearing and tearing, and the running speed of high-speed bearing is big, cause lubricant to be difficult for adhering to rolling surface, disperse easily, the rotational resistance of the bearing carrying roller of high-speed bearing is relatively large, therefore the lubricant that requires to be used for high-speed bearing possesses splendid anti-wear and wear-resistant performance, with the rotational resistance of the bearing carrying roller that reduces high-speed bearing, stick to the surface of bearing firmly, reduce the friction resistance between friction surface, prevent the wearing and tearing and the scratch of material, thereby cut down the consumption of energy and operation cost.The working temperature of high-speed bearing is mostly about 200 ℃, and tend to higher, common lithium saponify, sodium-base grease all can't satisfy the requirement of high temperature lubricating, because high-speed bearing is not as cooling off by powerful, then temperature can continue to rise and be greatly unfavorable to the intensity and the hardness of bearing, in a single day bearing loses the ability that keeps accurate shape, will aggravate high-speed friction and temperature is risen rapidly, further causes the reduction of the strength of materials and hardness and makes the very fast inefficacy of bearing.Therefore for high-speed bearing, select for use a kind of under hot environment, the synthetic oil lubricating oil that also has superperformance, or be that the lubricating grease of base oil is very necessary with this synthetic oil.
At present in the industry, polyurea based lubricating grease relies on its good temperature resistance, anti-radiation, water resisting property, colloid stability, and performance such as long bearing life and used producer to favor by great majority, development along with bearing technology, bearing progressively develops to closed type, sealing bearing requires lubricating grease work-ing life and same life-span of bearing usually, the centre is supplemental lubrication fat not, and bear high-speed bearing lubricated of huge impact and vibration, and other heavy duties, high loading, the operating mode of impact load, all need polyurea based lubricating grease to possess splendid anti-wear and wear-resistant performance and extreme pressure property can meet the demands, manyly in the industry at present achieve the goal to add oiliness improver or extreme pressure anti-wear additives.In order to reach splendid antifriction antiwear effect, general way is added multiple antiwear and friction-reducing additive at polyurea based lubricating grease often, and adding proportion is bigger, and so neither environmental protection is also uneconomical.
Summary of the invention
One object of the present invention is to overcome the deficiency of above-mentioned existence and a kind of high PB value, high-adhesiveness energy is provided; and have high dropping point polyurea based lubricating grease and preparation method; the present invention is by changing the adding technology of additive; additive is carried out the multiviscosisty reaction as the part of base oil; thereby the abrasion resistant extreme-pressure effect of additive is increased doubly; reduce the ratio of antiwear and friction-reducing additive, improved economic benefit, and helped environment protection.
A kind of high P provided by the invention
BThe polyurea based preparation of greases method of value comprises: at 50～80 ℃, preferred 60～70 ℃ add tackifier, part antiwear and friction-reducing additive in the base oil, dissolve, synthetic base oil, base oil after will synthesizing again is divided into three parts, wherein the mixture of two parts of base oils is used to dissolve vulcabond at 60～80 ℃ respectively, alkylamine, and portion is used as quenching oil in addition.Mix at 70～110 ℃ of two groups of solution after will dissolving, vigorous reaction, be warming up to fusion, add quenching oil, be cooled to 100～120 ℃, the abrasion resistant extreme-pressure additive that adds antioxidant preservative and remainder again, if needed, can also add functional additives such as extreme pressure agent, rust-preventive agent, continue to be cooled to 60～90 ℃, homogeneous goes out still.
The said base oil of the present invention can be selected the mineral oil of 400SN～650SN, and the mineral oil of high viscosity index (HVI) neutral oil, as bright stock 150BS, and synthesizing ester oil, a kind of in the vegetables oil, perhaps wherein two kinds, perhaps two or more mixtures.
In order to reach wideer use temperature scope and good adhesion property, and the effect that further improves antiwear and friction-reducing additive, in base oil, also need add tackifier, the said tackifier of the present invention can be selected a kind of in low-molecular-weight polyisobutene, polymethacrylate, the ethylene-propylene copolymer, or the mixture of two kinds or three kinds.In the present invention, tackifier account for 0～18% of lubricating grease total amount, and preferred 3～12%.
The said antiwear and friction-reducing additive of the present invention can be selected a kind of, two or the two or more mixtures in lipid acid, fatty amine, P contained compound friction improver, ester class friction improver, borate extreme-pressure anti-friction additive, the organic-molybdenum friction improver.
The said synthetic base oil of the present invention is the mixture of base oil, tackifier, antiwear and friction-reducing additive.The said synthetic base oil consumption of the present invention is 60～95% of a lubricating grease total amount, preferred 70～90%.Base oil after synthetic generally will be divided into three parts of addings, a copy of it is used to dissolve vulcabond, consumption is 50～70% of a synthetic base oil total amount, portion is used for dissolved fat amine in addition, consumption is 20～40% of a synthetic base oil total amount, the 3rd part of base oil adds at last as quenching oil, and consumption is 10～30% of a synthetic base oil total amount.
Viscosifying agent of the present invention is made of two carbamide compounds, and the carbamido thickening agent amount accounts for 5～20% of lubricating grease total amount, preferred 7-15%, and two carbamide compounds are by C
6～C
24Organic amine, preferred C
6～C
18Aliphatic amide and di-isocyanate reaction form, and vulcabond can be selected ditane-4,4-vulcabond or tolylene diisocyanate, preferred ditane-4,4-vulcabond.Described alkylamine can be a straight-chain fatty amine, also can be Cycloalkyl amine, and the consumption of alkylamine is a calculated value.
Adopt the high P of the present invention's preparation
BValue polyurea based lubricating grease also can add other additives, as required as rust-preventive agent, antioxidant preservative etc. in product.
Adopt the lubricating grease of the inventive method preparation to have following characteristics:
Superpower abrasion resistance, splendid portative power is specially adapted to that load is big, the operating mode of serious wear is lubricated;
Stronger adhesive ability and good water repelling property, bearing is extremely long work-ing life.
The lubricating grease of the present invention preparation can be used for the power lubrication of turning round under the bad working environments such as high temperature, heavy duty, humidity, hazardous medium and the bearing lubrication of high speed and ultrahigh speed running.
Embodiment
The present invention can make those skilled in the art more fully understand the present invention, but not limit the present invention in any way by the present invention of following specific embodiment more detailed description.
Embodiment 1
Getting 800g Xinjiang 150BS adds in the system fat still, in still, add the 50g molecular weight again and be 12000 polyisobutene, the 5g dimeracid, the 15g phosphoric acid ester, the star of 2g phosphorus, the 20g oleic acid glycol ester, be warming up to 60 ℃, constant temperature stirs 30min, again the synthetic base oil is divided into three parts, with weight is that first part of synthetic base oil of 600g places system fat still, in still, add 50gMDI (ditane-4, the 4-vulcabond), stirring heating is warming up to 70 ℃ and dissolves, accelerate to stir and constant temperature to 72 ℃ about, fill in the reactor of 200g synthetic base oil to another simultaneously and add the 20g tetradecy lamine, the 28g hexahydroaniline, and dissolving in the time of 60 ℃, under quick condition of stirring, the mixing solutions in the reactor is dropped in the system fat still fast, vigorous reaction takes place, when temperature rises to 115 ℃ in the system fat still, add remaining 92g synthetic base oil, continue to be warming up to 140 ℃, behind the insulation 10min, be cooled to 100 ℃, add 2% antioxidant preservative T202,0.5% phenyl-a-naphthylamines, 0.5% Span-80, constant temperature stirs 30min, be cooled to 80 ℃, homogeneous goes out still.Detected result is as shown in table 1.
Embodiment 2
Get 650g Xinjiang 150BS, the 150g rapeseed oil adds in the system fat still, in still, add 100gT603 again, 20g Tocp acid esters, 5g alkylphenol phosphorous acid ester, 10g dithiocarbamic acid molybdenum oxide, be warming up to 60 ℃, constant temperature stirs 30min, again the synthetic base oil is divided into three parts, with weight is that first part of synthetic base oil of 600g places system fat still, in still, add 50g MDI (ditane-4, the 4-vulcabond), stirring heating is warming up to 70 ℃ and dissolves, accelerate to stir and constant temperature to 72 ℃ about, fill in the reactor of 200g synthetic base oil to another simultaneously and add the 20g tetradecy lamine, the 28g hexahydroaniline, and dissolving in the time of 60 ℃, under quick condition of stirring, the mixing solutions in the reactor is dropped in the system fat still fast, vigorous reaction takes place, when temperature rises to 115 ℃ in the system fat still, add remaining 100g synthetic base oil, continue to be warming up to 140 ℃, behind the insulation 10min, be cooled to 100 ℃, add 2%T202,0.5% pentanoic, 3%T361A borate extreme-pressure anti-friction additive, constant temperature stirs 30min, be cooled to 80 ℃, homogeneous goes out still.Detected result is as shown in table 1.
Comparative Examples 1
Get 600g Xinjiang 150BS and add in the system fat still, give in the still again to add 50gMDI (ditane-4,4-vulcabond), stirring heating is warming up to 70 ℃ and dissolves, accelerate to stir and constant temperature to 72 ℃ about, fill in the reactor of 200g Xinjiang 150BS base oil to another simultaneously and add the 20g tetradecy lamine, the 28g hexahydroaniline, and dissolving in the time of 60 ℃, under quick condition of stirring, the mixing solutions in the reactor is dropped in the system fat still fast, vigorous reaction takes place, when temperature rises to 115 ℃ in the system fat still, add the 100g base oil, continue to be warming up to 140 ℃, behind the insulation 10min, be cooled to 100 ℃, add 20g T202,5g phenyl-a-naphthylamines, the 5g Span-80,50gT603, the 5g dimeracid, the 15g phosphoric acid ester, the star of 2g phosphorus, the 20g oleic acid glycol ester, constant temperature stirs 30min, be cooled to 80 ℃, homogeneous goes out still.Detected result is as shown in table 1.
Comparative Examples 2
Get 650g Xinjiang 150BS, the 150g rapeseed oil adds in the system fat still, in still, add 50gMDI (ditane-4, the 4-vulcabond), stirring heating is warming up to 70 ℃ and dissolves, accelerate to stir and constant temperature to 72 ℃ about, fill in the reactor of 200g synthetic base oil to another simultaneously and add the 20g tetradecy lamine, the 28g hexahydroaniline, and dissolving in the time of 60 ℃, under quick condition of stirring, the mixing solutions in the reactor is dropped in the system fat still fast, vigorous reaction takes place, when temperature rises to 115 ℃ in the system fat still, add remaining 100g synthetic base oil, continue to be warming up to 140 ℃, behind the insulation 10min, be cooled to 100 ℃, in still, add 100g T603,20g Tocp acid esters again, 5g alkylphenol phosphorous acid ester, 10g dithiocarbamic acid molybdenum oxide, 20g T202, the pentanoic of 5g, 30g T361A borate extreme-pressure anti-friction additive, constant temperature stirs 30min, be cooled to 80 ℃, homogeneous goes out still.Detected result is as shown in table 1.
Table 1
| Drawing cone in-degree (25 ℃) | Dropping point, ℃ | ??P BValue, kg | ??P DValue, kg | Corrosion (T 2Copper, 100 ℃, 24h) | |
| Embodiment 1 | ??301 | ??262 | ??141 | ??315 | Qualified |
| Embodiment 2 | ??304 | ??263 | ??135 | ??315 | Qualified |
| Drawing cone in-degree (25 ℃) | Dropping point, ℃ | ??P BValue, kg | ??P DValue, kg | Corrosion (T 2Copper, 100 ℃, 24h) | |
| Comparative Examples 1 | ??310 | ??255 | ??110 | ??250 | Qualified |
| Comparative Examples 2 | ??313 | ??256 | ??107 | ??250 | Qualified |
From table one as can be seen, the polyurea based lubricating grease that the tackifier that add same ratio by feature process of the present invention and antiwear and friction-reducing additive make is compared with the oilness of the lubricating grease that traditional additive adding technology makes, and the oilness of the polyurea based lubricating grease that the present invention makes has clear superiority.
The above is preferred embodiment of the present invention only, is not to be used for limiting practical range of the present invention, so all variations that is equal to according to feature raw material, characterization step and the prescription of scope of the present invention all should be included within the claim of the present invention.
Claims (9)
1. high P
BThe polyurea based preparation of greases method of value, comprise: tackifier, part antiwear and friction-reducing additive are dissolved in the base oil at 50～70 ℃, synthetic base oil, the base oil after will synthesizing again respectively with vulcabond, alkylamine mixes, react at 70～120 ℃, be warming up to fusion, add quenching oil, be cooled to 100～120 ℃, add antioxidant preservative, rust-preventive agent and remaining anti wear and friction reducing additives or other functional type additives, cool off still.
2. the described polyurea based lubricating grease of claim 1, it is characterized in that employed base oil is 100 ℃ of lubricating oil that viscosity is 20～50cst, described lubricating oil is to adopt a kind of in tackifier, mineral oil, synthetic oil, the vegetables oil or wherein two kinds, perhaps two or more mixtures.
3. the described synthetic base oil of claim 1 is characterized in that it being the mixture of described base oil of claim 3 and antiwear and friction-reducing additive.
4. the described polyurea based lubricating grease of claim 1, it is characterized in that employed synthetic base oil is divided into three parts of addings, a copy of it is used to dissolve vulcabond, consumption is 50～70% of a synthetic base oil total amount, portion is used for dissolved fat amine in addition, consumption is 20～40% of a synthetic base oil total amount, and a in addition base oil adds at last as quenching oil, and consumption is 10～30% of a synthetic base oil total amount.
5. the described polyurea based lubricating grease of claim 1 is characterized in that employed viscosifying agent is alicyclic urea, fatty urea or the mixture of the two.Carbamido thickening agent accounts for 5～20% of lubricating grease total amount, and two carbamide compounds are by C
6～C
24Organic amine, preferred C
6～C
18Aliphatic amide and di-isocyanate reaction form.Described vulcabond is a ditane-4,4-vulcabond or tolylene diisocyanate.
6. the described a kind of high P of claim 1
BThe polyurea based preparation of greases method of value is characterized in that this method is:
1), at first base oil is mixed in proportion, at 50～70 ℃ tackifier, part antiwear and friction-reducing additive are dissolved in the base oil synthetic base oil again;
2), the base oil after will synthesizing is according to the described proportional distribution of claim 4;
3), in accounting for 50～70% portion of synthetic base oil total amount, add vulcabond, 60～80 ℃ of dissolvings,, after 60～80 ℃ of dissolvings, add cycloalkanes amine again accounting for 20～40% the other a aliphatic amide that adds of synthetic base oil total amount, constant temperature evenly stirs at 65～75 ℃;
4), be 60～80 ℃ in temperature, above-mentioned two groups of solution are mixed, mixture reacts rapidly, is warming up to 105～120 ℃, adds the surplus synthetic base oil, continues to be warming up to 130～150 ℃ and carries out the high temperature refining, insulation 10～30min;
5), be cooled to 100～120 ℃, add antioxidant preservative and remaining anti wear and friction reducing additives or other functional type additives, continue to be cooled to 60～90 ℃, homogeneous goes out still.
7. the described polyurea based lubricating grease of claim 1, it is characterized in that described antiwear and friction-reducing additive is a kind of, two or the two or more mixture in lipid acid, fatty amine, P contained compound friction improver, ester class friction improver, borate extreme-pressure anti-friction additive, the organic-molybdenum friction improver, the ratio that additive accounts for the lubricating grease total amount is 2～8%.
8. the described polyurea based lubricating grease of claim 1 is characterized in that described tackifier are low-molecular-weight polyisobutene or polymethacrylate.
9. the described polyurea based lubricating grease of claim 1 is characterized in that the last non seizure load P of prepared lubricating grease in the time of 25 ℃
BValue is more than 135kg, and the cone penetration in the time of 25 ℃ is between the 220-340.
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| CN 200910236610 CN101696366B (en) | 2009-10-26 | 2009-10-26 | Method for preparing lubricating grease with excellent anti-wear and wear-resistant performance |
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| CN 200910236610 CN101696366B (en) | 2009-10-26 | 2009-10-26 | Method for preparing lubricating grease with excellent anti-wear and wear-resistant performance |
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| CN101696366A true CN101696366A (en) | 2010-04-21 |
| CN101696366B CN101696366B (en) | 2013-03-20 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101982533A (en) * | 2010-11-11 | 2011-03-02 | 侯亚君 | Antifriction antiwear liquid addition agent technology |
| CN105586135A (en) * | 2014-10-23 | 2016-05-18 | 中国石油化工股份有限公司 | Urea-based lubricating grease composition with excellent antifriction property and preparation method therefor |
| CN105838485A (en) * | 2016-04-13 | 2016-08-10 | 禾泰特种新材料（苏州）有限公司 | Grease composition and preparation method thereof |
| CN108004000A (en) * | 2017-12-26 | 2018-05-08 | 苏州贝尔纳德铁路设备有限公司 | A kind of track screw long-acting special anti-corrosion grease and preparation method thereof |
| CN109135886A (en) * | 2018-07-23 | 2019-01-04 | 中国铁路总公司 | A kind of high-speed EMUs antifriction-bearing grease composition and preparation method |
| CN110713859A (en) * | 2018-07-13 | 2020-01-21 | 中国石油天然气股份有限公司 | Diesel engine oil composition |
| CN111073732A (en) * | 2019-12-27 | 2020-04-28 | 辽宁海华科技股份有限公司 | Alkali-resistant lubricating grease and preparation method thereof |
| CN115287110A (en) * | 2022-08-02 | 2022-11-04 | 中科润美（青岛）材料科技有限公司 | Lubricating grease for high-speed high-temperature long-life angle grinder and preparation method thereof |
| CN116814318A (en) * | 2023-05-29 | 2023-09-29 | 新乡市恒星科技有限责任公司 | Lubricating grease special for bearing of drill grinder and preparation method thereof |
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| US5207935A (en) * | 1989-03-31 | 1993-05-04 | Amoco Corporation | Wheel bearing grease |
| US5223161A (en) * | 1989-06-27 | 1993-06-29 | Amoco Corporation | Extreme pressure and wear resistant grease with synergistic sulfate and carboxylate additive system |
| CN1657599A (en) * | 2004-02-18 | 2005-08-24 | 中国石油化工股份有限公司 | Polyurea grease composite |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101982533A (en) * | 2010-11-11 | 2011-03-02 | 侯亚君 | Antifriction antiwear liquid addition agent technology |
| CN105586135A (en) * | 2014-10-23 | 2016-05-18 | 中国石油化工股份有限公司 | Urea-based lubricating grease composition with excellent antifriction property and preparation method therefor |
| CN105586135B (en) * | 2014-10-23 | 2018-06-19 | 中国石油化工股份有限公司 | Excellent urea-based lubricating grease composition of a kind of Wear vesistance and preparation method thereof |
| CN105838485A (en) * | 2016-04-13 | 2016-08-10 | 禾泰特种新材料（苏州）有限公司 | Grease composition and preparation method thereof |
| CN105838485B (en) * | 2016-04-13 | 2019-08-06 | 埃优诺特种新材料科技(山东)有限公司 | Lubricant composition and preparation method thereof |
| CN108004000A (en) * | 2017-12-26 | 2018-05-08 | 苏州贝尔纳德铁路设备有限公司 | A kind of track screw long-acting special anti-corrosion grease and preparation method thereof |
| CN110713859A (en) * | 2018-07-13 | 2020-01-21 | 中国石油天然气股份有限公司 | Diesel engine oil composition |
| CN109135886A (en) * | 2018-07-23 | 2019-01-04 | 中国铁路总公司 | A kind of high-speed EMUs antifriction-bearing grease composition and preparation method |
| CN111073732A (en) * | 2019-12-27 | 2020-04-28 | 辽宁海华科技股份有限公司 | Alkali-resistant lubricating grease and preparation method thereof |
| CN111073732B (en) * | 2019-12-27 | 2021-12-10 | 辽宁海华科技股份有限公司 | Alkali-resistant lubricating grease and preparation method thereof |
| CN115287110A (en) * | 2022-08-02 | 2022-11-04 | 中科润美（青岛）材料科技有限公司 | Lubricating grease for high-speed high-temperature long-life angle grinder and preparation method thereof |
| CN116814318A (en) * | 2023-05-29 | 2023-09-29 | 新乡市恒星科技有限责任公司 | Lubricating grease special for bearing of drill grinder and preparation method thereof |
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Effective date of registration: 20170622 Address after: 062650 North Zone, Qingxian County Economic Development Zone, Hebei, Cangzhou Patentee after: Hebei nine hee new Mstar Technology Ltd Address before: 100043 West Street, Shijingshan District, Beijing, No. 19 Patentee before: Masuda Rissoil (Beijing) Chemicals Co., Ltd. |
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