CN101629121B - Novel lubricating grease and preparation method thereof - Google Patents
Novel lubricating grease and preparation method thereof Download PDFInfo
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- CN101629121B CN101629121B CN200910305542A CN200910305542A CN101629121B CN 101629121 B CN101629121 B CN 101629121B CN 200910305542 A CN200910305542 A CN 200910305542A CN 200910305542 A CN200910305542 A CN 200910305542A CN 101629121 B CN101629121 B CN 101629121B
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Abstract
The invention relates to novel lubricating grease and a preparation method thereof. A composite aluminum-urea based polyurea lubricating grease composition comprises the 85-95% of base oil and 5-15% of a gelling agent by weight percent. The gelling agent is a composition obtained from the reaction of an ingredient A and an ingredient B. The ingredient A is produced from the reaction of fatty acid of C16-C20, aromatic acid and organic aluminium with an equivalence ratio of 1:1-1.5:1. The ingredient B is produced from the reaction of isocyanate, alicyclic amine and aromatic amine with the equivalence ratio of 1:0.9-1.3:1.1-0.7. The gelling agent is formed by the reaction products of higher fatty acid in the ingredient A and the isocyanate in the ingredient B by taking the equivalence ratio of 0.5-1.5:1 as a standard. The preparation method of the lubricating grease is characterized by adopting one-step saponification compound process. Utilizing the proper material proportion, the lubricating grease has advantages of excellent high-temperature property with dropping point greater than 260 DEG C, simple process, energy saving, reduced production cost and stable quality of products.
Description
Technical field
The invention belongs to technical field of lubricating grease, particularly relate to a kind of novel lubricating grease and preparation method.
Background technology
Railway grease is divided into soap base grease and nonsoap grease usually, and wherein soap base grease is the most frequently used railway grease, no matter is that soap grease also is non-soap grease; The characteristics of railway grease itself are with variation of temperature; Grease consistency changes greatly, and high temperature grease particularly is though have higher dropping point (dropping point is greater than 300 ℃); But deliquescing loss of rising railway grease or hardening coking along with temperature have lost lubrication.General high temperature grease has composite aluminum base base grease and urea-base grease usually at present, and wherein deliquescing leakage (generally obvious in deliquescing more than 120 ℃, as leakage to occur) appears in composite aluminum base grease high temperature, causes that equipment lubrication lost efficacy; And urea-base grease, sclerosis appears in high temperature, and (according to different areidofats, its stiffening temperature is different; The hardened phenomenon generally appears in the time of 120～150 ℃); And along with the rising of temperature, hardening phenomenon is just obvious more, usually in the high temperature operation process, causes the stuck of running gear; Even cause the running gear sintering together, cause the shutdown of equipment.
Summary of the invention
The purpose of this invention is to provide a kind of railway grease, guaranteeing that its denseness has the characteristic that general railway grease has on the basis slowly with temperature variation with good thick warm nature ability.
Technology of the present invention is following:
The composition and the percentage composition of clad aluminum urea-based lubricating grease composition provided by the invention are following: base oil 85～95%, viscosifying agent 5～15%.
Viscosifying agent is that component A and B component reaction make compsn, and component A is by C
16～C
20Lipid acid, aromatic acid and organoaluminum with equivalence ratio be 1: 1～1.5: 1 the reaction make; B component is to be made with equivalence ratio 1: 0.9～1.3: 1.1～0.7 reaction by isocyanic ester, aliphatic amide and aromatic amine; The proportioning of component A and B component is to be benchmark resultant of reaction composition viscosifying agent at 0.5～1.5: 1 with the isocyanic ester of the higher fatty acid of A group and B component with equivalence ratio.
Described C
16～C
20Lipid acid comprise Triple Pressed Stearic Acid or ten dihydroxystearic acids;
Described aromatic acid comprises phenylformic acid or alkyl substituted benzoic acid;
Described organoaluminum comprises aluminum isopropylate or aluminium isopropoxide;
Described isocyanic ester comprises TDI (2, the 4-toluenediisocyanate) or MDI (4, the 4-diphenylmethanediisocyanate), HMDI (hexa-methylene-1,6-vulcabond);
Described aliphatic amide comprises octylame, amino dodecane or stearylamine;
Described aliphatic cyclic amine comprises hexahydroaniline;
The characteristics of the method for preparation of greases of the present invention are to adopt single stage method saponification recombining process, concrete steps:
(1) isocyanic ester of component B is added presses in the still oil, also joins in the base oil behind aliphatic amide and the aromatic amine proportional mixing; Be mixed and heated to 60～100 ℃; Add raw fatty acid, aromatic acid and the organoaluminum of forming component A in order in proportion; Carry out complex reaction, the reaction times is 1～2 hour.
(2) (1) step compound material is continued to be warming up to 100～140 ℃, add entry, water equivalent is the normal 2-4 of organoaluminum times, constant temperature 1～2 hour.
(3) (2) step compound material was continued to be warming up to 160～190 ℃ of constant temperature 0.5～1 hour.Add then and carry out aftertreatment after quenching oil stirs and promptly get required product.
Railway grease result of performance test of the present invention shows to have following advantage: owing to selected proper raw material proportioning for use; Make this railway grease have good properties at high temperature; Dropping point is greater than 260 ℃; Its outstanding advantage is that denseness obviously improves with temperature variation, and its denseness is not clearly with variation of temperature, can satisfy the use of wide temperature range.Compare with polyurea grease and to have the non-sclerous advantage of high temperature, have advantage cheaply simultaneously, compare with clad aluminum and have a good adhesion.Therefore railway grease of the present invention can be used for the bearing lubrication of high temperature services such as continuous casting, tandem rolling, square billet, slab.In addition, preparation of greases method of the present invention adopts the direct complex reaction of single stage method, thereby makes technology simple, and energy efficient has reduced production cost, and the quality product of this explained hereafter is also more stable.
Description of drawings
Fig. 1: railway grease of the present invention and existing capability of lubricating grease are relatively.
Embodiment
90 gram MDI are added in the pressure still oil of 1500 grams, be heated to 60 ℃, the aniline of the octylame of 45 grams and 35 grams is joined in the oil of 600 grams be heated to 60 ℃ simultaneously; Mix (these three kinds of raw material after chemical reactions generate the B component), add Triple Pressed Stearic Acid 51 grams, phenylformic acid 26 grams; Aluminium isopropoxide 18.4 grams rise to 90 ℃, constant temperature 1 hour (these three kinds of raw materials react at a certain temperature and generate the A component); Continue to be heated to 120 ℃, add 6.5 gram tap water, constant temperature 1 hour (B component and A component are further reacted and generated novel grease composition in this process); Continuation is warming up to 160 ℃ with material, and constant temperature 10 minutes (novel grease composition is further stable) adds quenching oil 700 grams; Carry out aftertreatment after stirring, the PERFORMANCE OF GREASES that technical recipe of the present invention makes is listed in table 1
Table 1
| Test subject | Sample 1# | Experimental technique |
| The Drawing cone in-degree, 0.1mm | 286 | GB/T269 |
| Dropping point, ℃ | 265 | GB/T3498 |
| Corrosion (100 ℃, 24h, T 2Cu) | Qualified | GB/T7326 second |
| The water pouring (79 ℃, 1h), loss amount, % | 0.01 | SH/T0109 |
Can know that by table 1 high-temperature behavior of railway grease of the present invention and water repelling property are all fine.
Material proportion is explained as follows:
Each raw material equivalence ratio in the A component: Triple Pressed Stearic Acid: phenylformic acid: aluminium isopropoxide is 1: 1.2: 1
Each raw material equivalence ratio: MDI in the B component: octylame: aniline is 1: 1: 1
The equivalence ratio of Triple Pressed Stearic Acid and MDI is 0.5: 1 for (being A component and B component equivalence ratio)
Viscosifying agent (quality of A+B) accounts for 8.1% of total railway grease amount
Adding the tap water equivalent is normal 2 times of aluminium isopropoxide.
The lab work of this instance is the Common item of the railway grease of chemical examination just, has the versatility that general railway grease has so that guarantee this fat.
Instance 2:
90 gram MDI are added in the pressure still oil of 1500 grams, be heated to 80 ℃, the hexahydroaniline of the amino dodecane of 66.8 grams and 34.6 grams is joined in the oil of 600 grams be heated to 80 ℃ simultaneously, mix; Add Triple Pressed Stearic Acid 102 grams, methyl-phenylformic acid 58.8 grams, aluminum isopropylate 73 grams; Constant temperature 1 hour continues to be heated to 100 ℃, adds 26 gram tap water; Constant temperature 1 hour continues material to be warming up to 170 ℃, constant temperature 0.5 hour; Add quenching oil 700 grams, carry out aftertreatment after stirring, the PERFORMANCE OF GREASES that technical recipe of the present invention makes is listed in table 2
Table 2
| Test subject | Sample 2# | Experimental technique |
| The Drawing cone in-degree, 0.1mm | 246 | GB/T269 |
| Dropping point, ℃ | 266 | GB/T3498 |
| Corrosion (100 ℃, 24h, T 2Cu) | Qualified | GB/T7326 second |
| The water pouring (79 ℃, 1h), loss amount, % | 0.01 | SH/T0109 |
Can know that by table 1 high-temperature behavior of railway grease of the present invention and water repelling property are all fine.
Material proportion is explained as follows:
Each raw material equivalence ratio in the A component: Triple Pressed Stearic Acid: methyl-phenylformic acid: aluminum isopropylate is 1: 1.2: 1
Each raw material equivalence ratio: MDI in the B component: amino dodecane: hexahydroaniline is 1: 1: 1
The equivalence ratio of Triple Pressed Stearic Acid and MDI is 1: 1 for (being A component and B component equivalence ratio).
Viscosifying agent (quality of A+B) accounts for 13.2% of total railway grease amount,
Adding from the beginning, the water yield is normal 2 times an of aluminum isopropylate
The lab work of this instance is the Common item of the railway grease of chemical examination just, has the versatility that general railway grease has so that guarantee this fat.
Instance 3:
28.4 gram TDI are added in the pressure still oil of 2600 grams, be heated to 100 ℃, the para-totuidine of the stearylamine of 48.5 grams and 19.3 grams is joined in the oil of 600 grams be heated to 100 ℃ simultaneously, mix; Add Triple Pressed Stearic Acid 77 grams, phenylformic acid 39 grams, aluminum isopropylate 55 grams are at 100 ℃; Constant temperature 1.2 hours continues to be heated to 140 ℃, adds 14.6 gram tap water, constant temperature 1.5 hours; Continuation is warming up to 190 ℃ with material, and constant temperature 30 minutes adds quenching oil 680 grams, carries out aftertreatment after stirring.The PERFORMANCE OF GREASES that technical recipe of the present invention makes is listed in table 3
Table 3
| Test subject | Sample 3# | Experimental technique |
| The Drawing cone in-degree, 0.1mm | 339 | GB/T269 |
| Dropping point, ℃ | 261 | GB/T3498 |
| Corrosion (100 ℃, 24h, T 2Cu) | Qualified | GB/T7326 second |
| The water pouring (79 ℃, 1h), loss amount, % | 0.02 | SH/T0109 |
Material proportion is explained as follows:
Each raw material equivalence ratio in the A component: Triple Pressed Stearic Acid: phenylformic acid: aluminum isopropylate is 1: 1.2: 1
Each raw material equivalence ratio: TDI in the B component: amino dodecane: hexahydroaniline is 1: 1: 1
The equivalence ratio of Triple Pressed Stearic Acid and TDI is 1.5: 1 for (being A component and B component equivalence ratio).
Viscosifying agent (quality of A+B) accounts for 7.5% of total railway grease amount,
Adding from the beginning, the water yield is normal 3 times an of aluminum isopropylate
The lab work of this instance is the Common item of the railway grease of chemical examination just, has the versatility that general railway grease has so that guarantee this fat,
Instance 4:
50 gram MDI are added in the pressure still oil of 2000 grams, be heated to 60 ℃, the hexahydroaniline of the stearylamine of 48.5 grams and 21.9 grams is joined in the oil of 1000 grams be heated to 60 ℃ simultaneously, mix; Add ten dihydroxystearic acids, 60 grams, phenylformic acid 24 grams, aluminum isopropylate 40.1 grams rise to 70 ℃; Constant temperature 1.5 hours continues to be heated to 120 ℃, adds 14.4 gram tap water, constant temperature 2 hours; Continuation is warming up to 170 ℃ with material, and constant temperature 1 hour adds quenching oil 1200 grams, carries out aftertreatment after stirring.The PERFORMANCE OF GREASES that technical recipe of the present invention makes is listed in table 3
Table 4
| Test subject | Sample 4# | Experimental technique |
| The Drawing cone in-degree, 0.1mm | 346 | GB/T269 |
| Dropping point, ℃ | 260 | GB/T3498 |
| Corrosion (100 ℃, 24h, T 2Cu) | Qualified | GB/T7326 second |
| The water pouring (79 ℃, 1h), loss amount, % | 0.03 | SH/T0109 |
Can know that by table 4 high-temperature behavior of railway grease of the present invention and water repelling property are all fine.
Material proportion is explained as follows:
Each raw material equivalence ratio in the A component: ten dihydroxystearic acids: phenylformic acid: aluminum isopropylate is 1: 1: 1
Each raw material equivalence ratio: MDI in the B component: stearylamine: hexahydroaniline is 1: 0.9:: 1.1
The equivalence ratio of ten dihydroxystearic acids and MDI is 1: 1 for (being A component and B component equivalence ratio).
Viscosifying agent (quality of A+B) accounts for 5.5% of total railway grease amount,
Adding from the beginning, the water yield is 4 times of aluminum isopropylate equivalents
The lab work of this instance is the Common item of the railway grease of chemical examination just, has the versatility that general railway grease has so that guarantee this railway grease.The characteristic of this railway grease is verified by Fig. 1.
Instance 5:
33.6 gram HMDI are added in the pressure still oil of 800 grams, be heated to 60 ℃, the hexahydroaniline of the stearylamine of 48.5 grams and 21.9 grams is joined in the oil of 200 grams be heated to 60 ℃ simultaneously, mix; Add Triple Pressed Stearic Acid 56.8 grams, phenylformic acid 36 grams, aluminum isopropylate 40.1 grams rise to 90 ℃; Constant temperature 2 hours continues to be heated to 120 ℃, adds 10.8 gram tap water, constant temperature 1 hour; Continuation is warming up to 170 ℃ with material, and constant temperature 1 hour adds quenching oil 350 grams, carries out aftertreatment after stirring.The PERFORMANCE OF GREASES that technical recipe of the present invention makes is listed in table 5
Table 5
| Test subject | Sample 5# | Experimental technique |
| The Drawing cone in-degree, 0.1mm | 226 | GB/T269 |
| Dropping point, ℃ | 265 | GB/T3498 |
| Corrosion (100 ℃, 24h, T 2Cu) | Qualified | GB/T7326 second |
| The water pouring (79 ℃, 1h), loss amount, % | 0.01 | SH/T0109 |
Can know that by table 5 high-temperature behavior of railway grease of the present invention and water repelling property are all fine.
Material proportion is explained as follows:
Each raw material equivalence ratio in the A component: Triple Pressed Stearic Acid: phenylformic acid: aluminum isopropylate is 1: 1.5: 1
Each raw material equivalence ratio: HMDI in the B component: stearylamine: hexahydroaniline is 1: 0.9:: 1.1
The equivalence ratio of Triple Pressed Stearic Acid and HMDI is 1: 1 for (being A component and B component equivalence ratio).
Viscosifying agent (quality of A+B) accounts for 14.9% of total railway grease amount.
Adding from the beginning, the water yield is normal 3 times an of aluminum isopropylate
Instance 6:
50 gram MDI are added in the pressure still oil of 2000 grams, be heated to 60 ℃, the hexahydroaniline of the stearylamine of 70.2 grams and 13 grams is joined in the oil of 600 grams be heated to 60 ℃ simultaneously, mix; Add Palmiticacid 51.8 grams, phenylformic acid 24 grams, aluminum isopropylate 40.1 grams rise to 75 ℃; Constant temperature 2 hours continues to be heated to 125 ℃, adds 9 gram tap water, constant temperature 2 hours; Continuation is warming up to 170 ℃ with material, and constant temperature 1 hour adds quenching oil 680 grams, carries out aftertreatment after stirring.The PERFORMANCE OF GREASES that technical recipe of the present invention makes is listed in table 6
Table 6
| Test subject | Sample 6# | Experimental technique |
| The Drawing cone in-degree, 0.1mm | 265 | GB/T269 |
| Dropping point, ℃ | 262 | GB/T3498 |
| Corrosion (100 ℃, 24h, T 2Cu) | Qualified | GB/T7326 second |
| The water pouring (79 ℃, 1h), loss amount, % | 0.03 | SH/T0109 |
Can know that by table 6 high-temperature behavior of railway grease of the present invention and water repelling property are all fine.
Material proportion is explained as follows:
Each raw material equivalence ratio in the A component: Palmiticacid: phenylformic acid: aluminum isopropylate is 1: 1.5: 1
Each raw material equivalence ratio: MDI in the B component: stearylamine: hexahydroaniline is 1: 1.3: 0.7
The equivalence ratio of Palmiticacid and MDI is 1: 1 for (being A component and B component equivalence ratio).
Viscosifying agent (quality of A+B) accounts for 7.1% of total railway grease amount
Adding from the beginning, the water yield is 2.5 times of the aluminum isopropylate equivalent thickness of aluminiums
Adopt the performance of railway grease and existing general railway grease and urea-base grease of present embodiment 1,2 and 3 more as shown in Figure 1.
Can find out from the thick warm nature variation diagram of scheming last three samples: (1) three sample is initial denseness difference, and it is identical with variation of temperature trend and velocity of variation, and this explains that we have good consistence aspect the thick warm nature ability at development product.(2) the thick warm nature of railway grease can have very big relation with the kind of viscosifying agent; General railway grease is with the rising denseness deliquescing always of temperature; Cause until not remaining on surface of friction pair running off, and urea-base grease with the rising of temperature 120 ℃ with interior deliquescing, denseness was with the quick hardening of the rising of temperature after temperature surpassed 120 ℃; Thereby cause lubrication failure, even cause the stuck of friction pair.(3) can find out that railway grease that we develop improves the thick warm nature of railway grease, is more suitable in the use of the wide temperature range of railway grease on scheme.
A kind of novel lubricating grease and preparation method that the present invention proposes; Be described through preferred embodiment; Person skilled obviously can be in not breaking away from content of the present invention, spirit and scope to component as herein described with method is changed or suitably change and combination, realize the present invention's technology.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as and are included in spirit of the present invention, scope and the content.
Claims (2)
1. a novel lubricating grease is characterized in that composition and quality percentage composition are base oil 85～95%, viscosifying agent 5～15%; Viscosifying agent is that component A and B component reaction make compsn, and component A is by C
16～C
20Lipid acid, aromatic acid and organoaluminum with mol ratio be 1: 1～1.5: 1 the reaction make; B component is to be made with mol ratio 1: 0.9～1.3: 1.1～0.7 reaction by isocyanic ester, aliphatic amide and aromatic amine; The proportioning of component A and B component is with the C of A group
16～C
20The isocyanic ester of lipid acid and B component be to be benchmark resultant of reaction form viscosifying agent at 0.5～1.5: 1 with mol ratio.
2. the preparation of greases method of claim 1 is characterized in that adopting single stage method saponification recombining process, concrete steps:
1) isocyanic ester of component B is added press in the still oil, aliphatic amide and aromatic amine proportional mixing join in the base oil; Be mixed and heated to 60～100 ℃; Add each raw material of forming component A; Add lipid acid, aromatic acid and organoaluminum in order in proportion, carry out complex reaction, the reaction times is 1～2 hour;
2) with 1) step compound material continues to be warming up to 100～140 ℃, adds entry, and the water yield is normal 2～4 times of organoaluminum, constant temperature 1～2 hour;
3) with 2) step compound material continued to be warming up to 160～190 ℃ of constant temperature 0.5～1 hour; Add then and carry out aftertreatment after quenching oil stirs and promptly get required product.
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| CN200910305542A CN101629121B (en) | 2009-08-12 | 2009-08-12 | Novel lubricating grease and preparation method thereof |
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| CN101629121B true CN101629121B (en) | 2012-08-29 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102002414A (en) * | 2010-10-13 | 2011-04-06 | 中国石油化工股份有限公司 | Polyurea lubricating grease composition |
| CN102268320B (en) * | 2011-07-07 | 2013-01-30 | 中国石油化工股份有限公司 | Food-grade lubricating grease as well as preparation method and application thereof |
| CN103484225A (en) * | 2013-08-29 | 2014-01-01 | 中国石油化工股份有限公司 | High-temperature polyurea lubricating grease composition and preparation method thereof |
| CN112375013B (en) * | 2020-11-18 | 2022-03-01 | 中国科学院兰州化学物理研究所 | Urea-based gel lubricant used in wide temperature range and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1493670A (en) * | 2002-10-30 | 2004-05-05 | 中国石油化工股份有限公司 | Ureido lubricating grease and its preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1493670A (en) * | 2002-10-30 | 2004-05-05 | 中国石油化工股份有限公司 | Ureido lubricating grease and its preparation method |
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Inventor after: Li Su Inventor after: Liu Qinglian Inventor after: Wu Baojie Inventor after: Gao Yanqing Inventor after: Li Dejing Inventor after: Dong Luhu Inventor after: Feng Yubao Inventor before: Li Su Inventor before: Liu Qinglian Inventor before: Wu Baojie Inventor before: Gao Yanqing Inventor before: Li Dejing Inventor before: Dong Luhu Inventor before: Feng Yubao |
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