CN1493673A - Preparation method of polyurea-composite calcium lubricating grease - Google Patents
Preparation method of polyurea-composite calcium lubricating grease Download PDFInfo
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- CN1493673A CN1493673A CNA021463840A CN02146384A CN1493673A CN 1493673 A CN1493673 A CN 1493673A CN A021463840 A CNA021463840 A CN A021463840A CN 02146384 A CN02146384 A CN 02146384A CN 1493673 A CN1493673 A CN 1493673A
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Abstract
A lubricating polyureas-composite calcium grease is prepared through proportionally mixing basic oil, calcium hydroxide (oxide), water and C1-C20 organic acid together, heating to 30-100 deg.C, adding diisocyanate and organic amine, draining water, saponifying, heating to 210-230 deg.C, cooling and homogenizing. Its advantages are high refractory performance, stability and extreme-pressure antiwear nature.
Description
Technical field
The present invention relates to the preparation of greases method.
Background technology
Polyureas-common preparation method of compound calcium mixed base grease prepares earlier two kinds of basic fat respectively, mixes by a certain percentage again.Provide a kind of method for preparing polyureas-compound calcium as CN1364859A, polyureas and compound calcium prepare respectively earlier, mix by a certain percentage again, complex procedures because lubricating grease viscosity is very big at normal temperatures, can't be used mechanical pump, change the still process by manually finishing, take time and effort.US 5,084, and 193 provide a kind of method for preparing polyureas-compound calcium grease, and prompting should be done polyurea grease earlier and do composite calcium-base fat again, also can prepare in reverse order, and be good but recommend last order.Yet when preparing polyureas-composite calcium-base fat according to last order, also have a problem, promptly after making polyurea grease, the temperature in the still has generally risen to 70-80 ℃, adds organic acid this moment more serious low molecular acid volatilization phenomenon can take place.
From above introduction as can be seen, during preparation polyureas-composite calcium-base fat, prior art is not advocated preparation composite calcium-base fat earlier, the method of refabrication polyurea grease, this may be owing to pot phenomenon that can rise in the process of preparation composite calcium-base fat, and promptly a large amount of foams rapid overflow in pot is in case this phenomenon occurs, defoamer must be added immediately, otherwise serious consequence can be caused.And those skilled in the art it is generally acknowledged and have been difficult in the same still preparation polyurea grease after pot phenomenon that rises.
Summary of the invention
The present invention overcomes the prejudice and the misleading of prior art, and a kind of direct method for preparing polyureas-complex calcium lubricating grease is provided.This method is preparation composite calcium-base fat earlier, does polyurea grease again, finishes in same still, not only can simplify the operation, and the polyureas-complex calcium lubricating grease that is obtained has more excellent characteristic.
Preparation of greases method of the present invention comprises: with base oil and calcium hydroxide (or calcium oxide), water and C
1-C
20Organic acid mixes, and is warming up to 30~100 ℃, adds vulcabond and organic amine, and the draining saponification is warmed up to 210~230 ℃, cooling, homogenizing.
Specifically, lubricating grease of the present invention can adopt following method preparation: at first the base oil with base oil gross weight 40~60% mixes in system fat still at normal temperatures with calcium hydroxide (or calcium oxide) and water, adds C then respectively
1-C
20Organic acid can be one or more acid, whenever add a kind of acid after, preferably reaction earlier adds another kind of acid after about 5~15 minutes again, after whole acid all adds, heats up.When temperature rises to 30~100 ℃, in the time of preferred 50~80 ℃,, pour in this still vulcabond heating for dissolving in 10~20% base oil, add C subsequently
8-C
24Organic amine, the draining saponification is until being warmed up to 210~230 ℃, add the surplus base oil, begin the circulation cooling, and in about 120 ℃, carry out homogenizing, homogenization pressures is generally 0.6~0.8MPa, and the homogenizing time obtains polyureas-composite calcium-base fat for being generally 10~50 minutes.Can in basic fat, add conventional additives as required, as oxidation inhibitor, rust-preventive agent etc.
Described base oil is mineral oil, ester class oil, synthetic hydrocarbon, plant wet goods.100 ℃ of viscosity are 20~40mm
2/ s is preferably 25~35mm
2/ s.
Said C
1-C
20Organic acid is selected from formic acid, acetate, propionic acid, phenylformic acid, diprotic acid, n-caprylic acid, boric acid, ten dihydroxystearic acids, stearic acid etc.Preferably select two kinds or two or more acid for use, generally select a kind of low molecular acid and a kind of polymer acid at least for use, select a kind of middle molecule acid (perhaps boric acid) in case of necessity again for use, it is generally acknowledged that the following acid of C6 is low molecular acid, the acid of C6-C10 is middle molecule acid, the above acid of C10 is polymer acid, and wherein the mol ratio of low molecular acid and polymer acid is 0.9~4: be advisable in 1 scope.
Said isocyanic ester is 4,4 '-diphenylmethanediisocyanate or 2, vulcabond such as 4-toluenediisocyanate.
Said carbon number is 8~24 preferred eight amine of organic amine, amino dodecane, cetylamine and stearylamine and cycloalkanes amine.
In the lubricating grease of the inventive method preparation (is benchmark with lubricating grease weight): base oil content is 50~90%, preferred 75~85%, viscosifying agent content is 10~50%, preferred 15~40%, described viscosifying agent comprises polyurea thickening agent and composite calcium-base viscosifying agent, wherein polyurea thickening agent is to be formed by organic amine and isocyanate reaction, and the composite calcium-base viscosifying agent is to be formed by organic acid and calcium hydroxide (or calcium oxide) reaction.The weight ratio of polyurea thickening agent and composite calcium-base viscosifying agent is 1: 0.3~3, preferred 1: 0.7~2.All determine consumption according to stoichiometric ratio between calcium hydroxide (or calcium oxide) and the organic acid and between vulcabond and the organic amine, the water yield is 1~5 times (weight) of calcium hydroxide (or calcium oxide).
Preparation method provided by the invention prepares composite calcium-base fat earlier, and the refabrication polyurea grease is not only easy and simple to handle, and has overcome the defective that prior art exists: owing to be to add organic acid under normal temperature even low temperature, can effectively avoid the volatilization of low molecular acid; Simultaneously add vulcabond and organic amine after adding organic acid but when also not rising pot, a pot phenomenon more just can not occur rising.In addition, polyureas-complex calcium lubricating grease that this method makes has excellent high-temperature performance, colloid stability, mechanical stability and extreme pressure anti-wear, can be used for high temperature, at a high speed, bearing lubrication such as heavy loading running, oil drilling.
Embodiment
Embodiment 1
With 800g 500SN oil (40 ℃ of viscosity, 100 ℃ of viscosity 11mm
2/ s) 94.5g calcium hydroxide and 450g water add in the normal oleosterin still, stir, and add the 117.9g Glacial acetic acid at normal temperatures, stir, and reacted about 10 minutes, add the 28.3g n-caprylic acid, stir, add ten dihydroxystearic acid 117.8g, heat to about 70 ℃.' diphenylmethanediisocyanate (MDI) 80.7g and 500SN oil 350g are heated to MDI and dissolve fully to add simultaneously 4,4 in container A.MDI oil solution in the container A is poured in the system fat still, heated to about 80 ℃.After this add amino dodecane 119.4g, the draining saponification continued to be warmed up to 220 ℃ after 2 hours, added the 200g quenching oil, stirred cooling, and the normal temperature grinding, got polyureas-composite calcium-base fat.Performance sees Table 1.
Embodiment 2
With 350g hydrogenation ﹠ Alpha ,-olefin oil (100 ℃ of viscosity 12mm
2/ s) add in the normal oleosterin still with 42g calcium hydroxide and 200g water, stir, add the 49g Glacial acetic acid at normal temperatures, stir, and reacted about 10 minutes, add 9.8g boric acid, stir, add ten dihydroxystearic acid 49g, heat to about 70 ℃.Simultaneously add 2 in container A, 4-toluenediisocyanate (TDI) 28g and base oil 150g are heated to MDI and dissolve fully.MDI oil solution in the container A is poured in the system fat still, heated to about 80 ℃.After this add amino dodecane 59.7g, the draining saponification continued to be warmed up to 220 ℃ after 2 hours, added the 100g quenching oil, stirred cooling, and the normal temperature grinding, got polyureas-composite calcium-base fat.Performance sees Table 1.
Embodiment 3
With 450g pentaerythritol ester (100 ℃ of viscosity 12mm
2/ s) add in the normal oleosterin still with 42g calcium hydroxide and 200g water, stir, add the 49g Glacial acetic acid at normal temperatures, stir, and reacted about 10 minutes, add the 12g n-caprylic acid, stir, add ten dihydroxystearic acid 49g, heat to about 70 ℃.' diphenylmethanediisocyanate (MDI) 42g and base oil 150g are heated to MDI and dissolve fully simultaneously to add 4,4 in container A.MDI oil solution in the container A is poured in the system fat still, heated to about 80 ℃.After this add stearylamine 90g, the draining saponification continued to be warmed up to 220 ℃ after 2 hours, added the 70g quenching oil, stirred cooling, and the normal temperature grinding, got polyureas-composite calcium-base fat.Performance sees Table 1.
Comparative Examples 1
According to the CN1364859A disclosed method, prepare polyureas and composite calcium-base fat respectively, mix by a certain percentage again.
With 2.7kg 500SN oil 2.7kg 150BS oil, 0.8kg calcium hydroxide and 3Kg water add among the normal pressure still A, stir, add the 0.9kg Glacial acetic acid at normal temperatures, stir, and reacted about 10 minutes, add 0.2kg boric acid, stir, add ten dihydroxystearic acid 0.9kg, heat to about 100 ℃, water is discharged, add 1.3kg 500SN oil and 1.3kg 150SN oil at last, continue to be warmed up to 220 ℃, circulation cooling, and normal temperature grinding get calcium grease.
Stearylamine 1.2kg and 150BS oil 4.1kg are added among the normal pressure still B, and be heated to 70 ℃, in container C, add vulcabond (MDI) 0.6kg and 500SN oil 4.1kg simultaneously, be heated to MDI and dissolve fully.MDI oil solution in the container C is poured in the still, stirred, add entry 300g, heat to 180 ℃, constant temperature 1 hour, circulation cooling and normal temperature grind, and get areidofat.
Calcium grease 200g is mixed with areidofat 200g, and stirring promptly gets grease product.Performance sees Table 1.
Comparative Examples 2
This example is the preparation polyurea grease earlier, refabrication composite calcium-base fat.
' diphenylmethanediisocyanate (MDI) 60.5g and 500SN oil 450g are heated to MDI and dissolve fully to add 4,4 in container A.MDI oil solution in the container A is poured in the system fat still that is added with 500SN 700g base oil and 89.5g amino dodecane, heated to about 80 ℃, stir fast.After this add calcium hydroxide 53.83g and 150g water, temperature is reduced to 40 ℃, add Glacial acetic acid 66.9g, 70 ℃ add sad 16.1g, and 80 ℃ add 12 oxystearic acid 66.9g, after the draining saponification 2 hours, continue to be warmed up to 220 ℃, add quenching oil 200g, stir cooling, and the normal temperature grinding, get polyureas-composite calcium-base fat.Performance sees Table 1.
The physicochemical property of table 1 lubricating grease
As can be seen from Table 1, the lubricating grease of the inventive method preparation is compared with reference fat, has higher dropping point, more favorable mechanical stability, colloid stability and excellent extreme pressure and antiwear behavior.
Claims (10)
1. the preparation method of polyureas-compound calcium grease comprises: with base oil and calcium hydroxide or calcium oxide, water and C
1-C
20Organic acid mixes, and is warming up to 30~100 ℃, adds vulcabond and organic amine, and the draining saponification is warmed up to 210~230 ℃, cooling, homogenizing.
2. according to the described preparation method of claim 1, it is characterized in that, at first 40~60% base oil and calcium hydroxide or calcium oxide and water are mixed at normal temperatures, add C
1-C
20Organic acid, temperature rise to 50~80 ℃, pour the vulcabond that is dissolved in 10~20% the base oil into, and add C
8-C
24Organic amine, the draining saponification is warmed up to 210~230 ℃, adds the surplus base oil, the circulation cooling, homogenizing, homogenization pressures are 0.6~0.8MPa, the homogenizing time is 10~50 minutes, obtains polyureas-compound calcium grease fat.
3. according to claim 1 or 2 described preparation methods, it is characterized in that, add additive in the cooling homogenizing stage.
4. according to claim 1 or 2 described preparation methods, it is characterized in that said base oil is selected from mineral oil, ester class oil, synthetic hydrocarbon and vegetables oil, 100 ℃ of viscosity are 20~40mm
2/ s.
5. according to claim 1 or 2 described preparation methods, it is characterized in that said C
1-C
20Organic acid is selected from formic acid, acetate, propionic acid, phenylformic acid, diprotic acid, n-caprylic acid, boric acid, ten dihydroxystearic acids and stearic acid.
6. according to claim 1 or 2 described preparation methods, it is characterized in that said organic acid is selected from a kind of C at least
6Following low molecular acid and a kind of C
10-C
20Above polymer acid, wherein the mol ratio of low molecular acid and polymer acid is 0.9~4: 1.
7. according to claim 1 or 2 described preparation methods, it is characterized in that, said isocyanic ester is 4,4 '-diphenylmethanediisocyanate or 2, the 4-toluenediisocyanate.
8. according to claim 1 or 2 described preparation methods, it is characterized in that said carbon number is that 8~24 organic amine is selected from eight amine, amino dodecane, cetylamine, stearylamine and cycloalkanes amine.
9. according to claim 1 or 2 described preparation methods, it is characterized in that, is benchmark with lubricating grease weight, and base oil content is 50~90%, and viscosifying agent content is 10~50%, and the weight ratio of polyurea thickening agent and composite calcium-base viscosifying agent is 1: 0.3~3.
10. according to the described preparation method of claim 9, it is characterized in that base oil content is 75~85%, viscosifying agent content is 15~40%, and the weight ratio of polyurea thickening agent and composite calcium-base viscosifying agent is 1: 0.7~2.
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CN108865373B (en) * | 2018-08-05 | 2021-08-17 | 杭州新港润滑科技有限公司 | Composite calcium sulfonate polyurea mixed lubricating grease and preparation method thereof |
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