CN101629121A - Novel lubricating grease and preparation method thereof - Google Patents
Novel lubricating grease and preparation method thereof Download PDFInfo
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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
Lubricating grease is divided into soap base grease and nonsoap grease usually, wherein soap base grease is the most frequently used lubricating grease, no matter be that soap grease also is non-soap grease, the characteristics of lubricating 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 lubricating 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; high temperature sclerosis occurs (according to different areidofats; its stiffening temperature difference; 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 causes the stuck of running gear in the high temperature operation process; 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 have good thick warm nature can lubricating grease, guaranteeing that its denseness varies with temperature slowly and has the characteristic that general lubricating grease has on the basis.
Technology of the present invention is as follows:
The composition and the percentage composition of clad aluminum urea-based lubricating grease composition provided by the invention are as follows: base oil 85～95%, viscosifying agent 5～15%.
Viscosifying agent is that component A and B component reaction make composition, 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 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 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 press in the still oil, aliphatic amide and aromatic amine also join in the base oil after being mixed in proportion, 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.
Lubricating 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 lubricating grease have good properties at high temperature, dropping point is greater than 260 ℃, its outstanding advantage is that denseness varies with temperature obviously and improves, 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 lubricating grease of the present invention can be used for the bearing lubrication of high temperature equipment 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: lubricating 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 ℃, simultaneously with 45 the gram octylames and 35 the gram aniline join 600 the gram oil in be heated to 60 ℃, mix (these three kinds of raw material after chemical reactions generate the B component), add 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) continues to be heated to 120 ℃, adds 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 evenly, 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 |
As shown in Table 1, the high-temperature behavior of lubricating grease of the present invention and water repelling property are all fine.
Material proportion is described as follows:
Each raw material equivalence ratio in the A component: 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 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 lubricating grease amount
Adding the tap water equivalent is normal 2 times of aluminium isopropoxide.
The lab work of this example is the Common item of the lubricating grease of chemical examination just, has the versatility that general lubricating grease has so that guarantee this fat.
Example 2:
90 gram MDI are added in the pressure still oil of 1500 grams, be heated to 80 ℃, simultaneously with 66.8 the gram amino dodecanes and 34.6 the gram hexahydroaniline join 600 the gram oil in be heated to 80 ℃, mix, add stearic acid 102 grams, tolyl acid 58.8 grams, aluminum isopropylate 73 grams, constant temperature 1 hour, continue to be heated to 100 ℃, add 26 gram tap water, constant temperature 1 hour continues material is warming up to 170 ℃, constant temperature 0.5 hour, add quenching oil 700 grams, carry out aftertreatment after stirring evenly, 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 |
As shown in Table 1, the high-temperature behavior of lubricating grease of the present invention and water repelling property are all fine.
Material proportion is described as follows:
Each raw material equivalence ratio in the A component: stearic acid: tolyl 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 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 lubricating grease amount,
Adding from the beginning, the water yield is normal 2 times an of aluminum isopropylate
The lab work of this example is the Common item of the lubricating grease of chemical examination just, has the versatility that general lubricating grease has so that guarantee this fat.
Example 3:
28.4 gram TDI are added in the pressure still oil of 2600 grams, be heated to 100 ℃, simultaneously the para-totuidine of the stearylamines of 48.5 grams and 19.3 grams are joined in the oil of 600 grams and be heated to 100 ℃, mix, add stearic acid 77 grams, phenylformic acid 39 grams, aluminum isopropylate 55 grams, at 100 ℃, constant temperature 1.2 hours, continue to be heated to 140 ℃, add 14.6 gram tap water, constant temperature 1.5 hours, continuation is warming up to 190 ℃ with material, 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 described as follows:
Each raw material equivalence ratio in the A component: 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 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 lubricating grease amount,
Adding from the beginning, the water yield is normal 3 times an of aluminum isopropylate
The lab work of this example is the Common item of the lubricating grease of chemical examination just, has the versatility that general lubricating grease has so that guarantee this fat,
Example 4:
50 gram MDI are added in the pressure still oil of 2000 grams, be heated to 60 ℃, simultaneously the hexahydroaniline of the stearylamines of 48.5 grams and 21.9 grams are joined in the oil of 1000 grams and be heated to 60 ℃, mix, add ten dihydroxystearic acids, 60 grams, phenylformic acid 24 grams, aluminum isopropylate 40.1 grams rise to 70 ℃, constant temperature 1.5 hours, continue to be heated to 120 ℃, add 14.4 gram tap water, constant temperature 2 hours, continuation is warming up to 170 ℃ with material, 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 |
As shown in Table 4, the high-temperature behavior of lubricating grease of the present invention and water repelling property are all fine.
Material proportion is described 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 lubricating grease amount,
Adding from the beginning, the water yield is 4 times of aluminum isopropylate equivalents
The lab work of this example is the Common item of the lubricating grease of chemical examination just, has the versatility that general lubricating grease has so that guarantee this lubricating grease.The characteristic of this lubricating grease is verified by Fig. 1.
Example 5:
33.6 gram HMDI are added in the pressure still oil of 800 grams, be heated to 60 ℃, simultaneously the hexahydroaniline of the stearylamines of 48.5 grams and 21.9 grams are joined in the oil of 200 grams and be heated to 60 ℃, mix, add stearic acid 56.8 grams, phenylformic acid 36 grams, aluminum isopropylate 40.1 grams rise to 90 ℃, constant temperature 2 hours, continue to be heated to 120 ℃, add 10.8 gram tap water, constant temperature 1 hour, continuation is warming up to 170 ℃ with material, 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 |
As shown in Table 5, the high-temperature behavior of lubricating grease of the present invention and water repelling property are all fine.
Material proportion is described as follows:
Each raw material equivalence ratio in the A component: 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 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 lubricating grease amount.
Adding from the beginning, the water yield is normal 3 times an of aluminum isopropylate
Example 6:
50 gram MDI are added in the pressure still oil of 2000 grams, be heated to 60 ℃, simultaneously the hexahydroaniline of the stearylamines of 70.2 grams and 13 grams are joined in the oil of 600 grams and be heated to 60 ℃, mix, add Palmiticacid 51.8 grams, phenylformic acid 24 grams, aluminum isopropylate 40.1 grams rise to 75 ℃, constant temperature 2 hours, continue to be heated to 125 ℃, add 9 gram tap water, constant temperature 2 hours, continuation is warming up to 170 ℃ with material, 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 |
As shown in Table 6, the high-temperature behavior of lubricating grease of the present invention and water repelling property are all fine.
Material proportion is described 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 lubricating grease amount
Adding from the beginning, the water yield is 2.5 times of the aluminum isopropylate equivalent thickness of aluminiums
The performance that adopts the lubricating grease of present embodiment 1,2 and 3 and existing general lubricating grease and urea-base grease more as shown in Figure 1.
From the thick warm nature variation diagram of scheming last three samples as can be seen: (1) three sample is initial denseness difference, and it is identical with variation of temperature trend and velocity of variation, this illustrate our development product thick warm nature can aspect have good consistence.(2) the thick warm nature of lubricating grease can have very big relation with the kind of viscosifying agent, general lubricating grease is with the rising denseness deliquescing always of temperature, cause running off until not remaining on surface of friction pair, and urea-base grease with the rising of temperature at 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) from the figure as can be seen the lubricating grease of our development the thick warm nature of lubricating grease is improved, be more suitable in the use of the wide temperature range of lubricating grease.
A kind of novel lubricating grease and preparation method that the present invention proposes, be described by 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 technology of the present invention.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 being included in spirit of the present invention, scope and the content.
Claims (3)
1. a novel lubricating grease is characterized in that composition and quality percentage composition are as follows: base oil 85～95%, viscosifying agent 5～15%.
2. lubricating grease as claimed in claim 1 is characterized in that viscosifying agent is that the reaction of component A and B component makes composition, and component A is to be that reaction in 1: 1～1.5: 1 makes by the lipid acid of C16～C20, aromatic acid and organoaluminum with mol ratio; 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 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 mol ratio.
3. the preparation method of claim 1 or 2 novel lubricating grease 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 be mixed in proportion and 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 the 10-30% of the quality of aluminum isopropylate, 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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|---|---|---|---|
| CN200910305542A CN101629121B (en) | 2009-08-12 | 2009-08-12 | Novel lubricating grease and preparation method thereof |
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| CN101629121A true CN101629121A (en) | 2010-01-20 |
| CN101629121B CN101629121B (en) | 2012-08-29 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002414A (en) * | 2010-10-13 | 2011-04-06 | 中国石油化工股份有限公司 | Polyurea lubricating grease composition |
| CN102268320A (en) * | 2011-07-07 | 2011-12-07 | 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 |
| CN112375013A (en) * | 2020-11-18 | 2021-02-19 | 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1239685C (en) * | 2002-10-30 | 2006-02-01 | 中国石油化工股份有限公司 | Ureido lubricating grease and its preparation method |
-
2009
- 2009-08-12 CN CN200910305542A patent/CN101629121B/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002414A (en) * | 2010-10-13 | 2011-04-06 | 中国石油化工股份有限公司 | Polyurea lubricating grease composition |
| CN102268320A (en) * | 2011-07-07 | 2011-12-07 | 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 |
| CN112375013A (en) * | 2020-11-18 | 2021-02-19 | 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 |
| 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 |
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| CN101629121B (en) | 2012-08-29 |
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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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