CN102911761B - High-temperature-resistant extreme pressure type lubricating grease composition and preparation method - Google Patents
High-temperature-resistant extreme pressure type lubricating grease composition and preparation method Download PDFInfo
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Abstract
The invention relates to a high-temperature-resistant extreme pressure type lubricating grease composition and a preparation method of the high-temperature-resistant extreme pressure type lubricating grease composition. The preparation method comprises steps as follows: mixing high-base-value calcium naphthenate, high-base-value sulfoacid calcium, and 35 to 65% of base oil; agitating; then adding a transforming agent; heating to reach 75 to 105 DEG C; maintaining the temperature for 40 to 120 minutes until the materials are thick; continuously heating the material until the temperature reaches more than 200 DEG C; removing the water completely, wherein the rest base oil is added during heating; continuously heating the materials until the temperature reaches 220 to 240 DEG C; agitating for 5 to 30 minutes at constant temperature until the materials are thick; and cooling and homogenizing to obtain the product as requirements. The lubricating grease prepared by the preparation method is high in comprehensive performance, excellent in high-temperature resistance, and high in extreme-pressure wear resistance, and can be used for lubricating high-temperature equipment with high load; and the requirements on use in high-temperature and high-load lubricating situations in the ferrous metallurgy industry can be met.
Description
Technical field
The invention belongs to technical field of lubricating grease, particularly relating to a kind of basicity calcium naphthenate that adopts is the high temperature resistant extreme pressure type composition that main raw material is crowded into fat.
Background technology
The present invention relates to a kind of basicity calcium naphthenate that adopts is the new grease composition that main raw material is crowded into fat, and it needn't add additive, and basic fat itself have outstanding high thermal resistance and good extreme pressure anti-wear etc.
Existing premium quality product complex calcium sulfonate grease is to take alkaline sulfoacid calcium as main raw material, and main raw material of the present invention is basicity calcium naphthenate, and alkaline sulfoacid calcium contents is less.Other is high temperature resistant lubricating grease, as products such as polyurea grease, compositing lithio ester, aluminum complex greases, need add some extreme pressure anti-wear additives just can have good extreme pressure anti-wear conventionally.At present, finding no employing basicity calcium naphthenate is the bibliographical information that main raw material makes lubricating grease.Basicity calcium naphthenate is also a kind of detergent for lubricating oil, generally by naphthenic acid (claiming again petroleum acid), makes, and naphthenic acid is the by product of refining of petroleum, and raw material is easy to get.
The present invention is directed to the lubricated occasion (sending roller-way, straightener etc. as steel billet heat) of iron and steel metallurgy industry high temperature higher load, by screening suitable composition and engineering, developing a kind of basicity calcium naphthenate that adopts is the new high-performance lubricating grease composition with outstanding high thermal resistance and good extreme pressure anti-wear that main raw material is crowded into fat.
Summary of the invention
The object of the present invention is to provide a kind of formula and preparation method of the new grease composition with outstanding high thermal resistance and extreme pressure anti-wear.The present invention makes a kind of new grease composition by lot of experiments screening formula and technique, meets the service requirements of the lubricated occasion of iron and steel metallurgy industry high temperature higher load.
Technology of the present invention is as follows:
A high temperature resistant extreme-pressure lubricating grease composition, its component and quality percentage composition are as follows:
(1) content of the high base number calcium naphthenate that base number is 250～420mgKOH/g is 30～60%;
(2) content of the calcium sulfonate with high base number that base number is 350～420mgKOH/g is 5～20%;
(3) lubricating base oil, surplus.
Commercially available high base number calcium naphthenate and calcium sulfonate with high base number all belong to Newtonian fuid, wherein contain amorphous calcium carbonate, by its characteristic peak of infrared measurement, are 860cm
-1left and right.Under the effect of transforming agent, amorphous calcium carbonate changes crystal habit into and exists, and by infrared measurement, obtains characteristic peak at 870～876cm
-1left and right, is mainly vaterite-type calcium carbonate crystal, and now material is converted into non-newtonian fluid by newton's body.And during to end product, be still also vaterite-type crystallization.
Transforming agent is in early stage, in conversion process, to add for promoting the conversion of calcium carbonate crystal formation, and in last handling process, major part has been overflowed from system, therefore excludes in component.
The base number of described high base number calcium naphthenate is 250～420mgKOH/g, preferred 280～420mgKOH/g, and quality percentage composition is 30～60%, preferably 30～50%; The base number of described calcium sulfonate with high base number is 350～420mgKOH/g, preferred 380～420mgKOH/g, and quality percentage composition is 5～20%, preferably 5～15%.
Described lubricating base oil can be mineral oil, alkene synthetic oil or the mixture of the two, 100 ℃ of kinematic viscosity 10～60mm
2/ s, open flash point is greater than 240 ℃.
The concrete steps of high temperature resistant extreme-pressure lubricating grease preparation method of composition of the present invention are as follows:
(1) high base number calcium naphthenate, calcium sulfonate with high base number, 35～65% base oil are mixed, after stirring, add transforming agent, be warming up to 75～105 ℃, preferably 80～100 ℃, keep 40～120min, to material retrogradation.With Fourier infrared spectrograph, be determined at 870～876cm
-1there is the absorption peak of vaterite-type calcium carbonate left and right.
Transforming agent can (before 75～105 ℃ of thermostatic processes) add in stirring temperature-rise period.
High base number calcium naphthenate itself transforms more difficult, introduces after a small amount of calcium sulfonate with high base number, has solved this difficult problem.
Described transforming agent comprises the alkyl benzene sulphonate (ABS) of lipid acid, fatty alcohol of C1～C5 etc. and C8～C15 and water etc., two or more the mixture wherein such as preferable formic acid, acetic acid, propionic acid, ethanol, Virahol, n-propyl alcohol, propyl carbinol, Witco 1298 Soft Acid or water.
(2) material of (1) step gained is continued to be warming up to 200 ℃ above by water emptying, in temperature-rise period, surplus base oil is added;
(3) material of (2) step is continued to be warming up to 220 ℃～240 ℃, constant temperature stirs 5～30 minutes, and after material retrogradation, cooling homogenizing obtains required product.
The equipment lubrication position of iron and steel metallurgy industry high temperature higher load is more, the present invention is as a kind of new high temperature resistant extreme-pressure lubricating grease, because raw material high base number calcium naphthenate is lower than calcium sulfonate with high base number, therefore grease product cost will be lower than calcium sulphonate type grease product, thereby has good application prospect at steel industry.
Embodiment
In order to screen suitable composition and engineering, in laboratory, experienced repeatedly failed case, at this, select the evaluation that several examples of many successful have been carried out high thermal resistance and extreme pressure anti-wear.
Effect of the present invention further illustrates by the following examples.But should understand, the following examples do not limit the scope of the invention, any change that does not exceed design of the present invention and scope, all within the scope of the present invention.
Embodiment 1:
The sulfonate with high base number acid calcium that the high base number calcium naphthenate that is 410mgKOH/g by 140g base number and 60g base number are 400mgKOH/g adds in 100g mineral oil, be heated with stirring to 50～60 ℃, add 10g propyl carbinol and 30g water, continue to heat up and be stirred to 80～90 ℃, add 20g acetic acid, material retrogradation after constant temperature 40min, infrared detection has 874cm
-1absorption peak.Continue to stir intensification draining, add 120g mineral oil after being heated to 200 ℃.Then, be further heated with stirring to 225～235 ℃, material is retrogradation gradually, and after constant temperature 5～10min, the homogenizing that cools makes finished product lubricating grease.Lubricating grease mass percent consists of: high base number calcium naphthenate 33.3%, calcium sulfonate with high base number 14.3%, base oil 52.4%.Prepared PERFORMANCE OF GREASES is listed in table 1.
Embodiment 2:
The calcium sulfonate with high base number that the high base number calcium naphthenate that is 420mgKOH/g by 160g base number and 40g base number are 380mgKOH/g adds in 100g mineral oil, heated and stirred to 85～95 ℃, add 25g water and 24g acetic acid, material retrogradation gradually after slowly stirring, after constant temperature 60min, infrared detection has 875cm
-1absorption peak.Continue to stir intensification draining, add 90g mineral oil after being heated to 170～180 ℃.Then, be further heated with stirring to 225～235 ℃, material is retrogradation gradually, and after constant temperature 10～15min, the homogenizing that cools makes finished product lubricating grease.Lubricating grease mass percent consists of: high base number calcium naphthenate 41.0%, calcium sulfonate with high base number 10.3%, base oil 48.7%.Prepared PERFORMANCE OF GREASES is listed in table 1.
Embodiment 3:
The calcium sulfonate with high base number that the high base number calcium naphthenate that is 310mgKOH/g by 150g base number, 50g base number are 410mgKOH/g adds in 80g alkene synthetic oil, stirring is warming up to after 70～80 ℃, add 15g Virahol, 20g water, 35g Witco 1298 Soft Acid, material retrogradation gradually after continuing to be heated to 90～100 ℃, after constant temperature 70min, infrared detection has 875cm
-1absorption peak.Continue to stir intensification draining, add 80g alkene synthetic oil after being heated to 190 ℃.Then, be further heated with stirring to 230～240 ℃, material is retrogradation gradually, and after constant temperature 20～30min, the homogenizing that cools makes finished product lubricating grease.Lubricating grease mass percent consists of: high base number calcium naphthenate 41.7%, calcium sulfonate with high base number 13.9%, base oil 44.4%.Prepared PERFORMANCE OF GREASES is listed in table 1.
Embodiment 4:
The calcium sulfonate with high base number that the high base number calcium naphthenate that is 280mgKOH/g by 120g base number, 80g base number are 350mgKOH/g adds in 100g mineral oil, stirring is warming up to after 70～80 ℃, add 10g Virahol, 20g water, 15g propionic acid, material retrogradation gradually after continuing to be heated to 90～100 ℃, after constant temperature 120min, continue to stir intensification draining, add 100g mineral oil after being heated to 190 ℃.Then, be further heated with stirring to 230～240 ℃, material is retrogradation gradually, and after constant temperature 20～30min, the homogenizing that cools makes finished product lubricating grease.Lubricating grease mass percent consists of: high base number calcium naphthenate 30%, calcium sulfonate with high base number 20%, base oil 50%.Prepared PERFORMANCE OF GREASES is listed in table 1.
Embodiment 5:
The calcium sulfonate with high base number that the high base number calcium naphthenate that is 250mgKOH/g by 240g base number, 20g base number are 420mgKOH/g adds in 90g mineral oil, after stirring, add 25g ethanol, 85g Witco 1298 Soft Acid, be heated to 85～95 ℃, constant temperature 120min, material retrogradation, then continue to stir intensification draining, adds 50g alkene synthetic oil after being heated to 180 ℃.Then, be further heated with stirring to 230～240 ℃, material is retrogradation gradually, and after constant temperature 10～15min, the homogenizing that cools makes finished product lubricating grease.Lubricating grease mass percent consists of: high base number calcium naphthenate 60%, calcium sulfonate with high base number 5%, base oil 35%.Prepared PERFORMANCE OF GREASES is listed in table 1.
Embodiment 6:
The calcium sulfonate with high base number that the high base number calcium naphthenate that is 400mgKOH/g by 200g base number, 40g base number are 400mgKOH/g adds in 60g mineral oil, stirring is warming up to after 60～70 ℃, add 20g water, 15g formic acid, continue to be heated to 75～85 ℃, constant temperature 100min, material retrogradation, then continue to stir intensification draining, adds 100g mineral oil after being heated to 170 ℃.Then, be further heated with stirring to 220～230 ℃, material is retrogradation gradually, and after constant temperature 5～10min, the homogenizing that cools makes finished product lubricating grease.Lubricating grease mass percent consists of: high base number calcium naphthenate 50%, calcium sulfonate with high base number 10%, base oil 40%.Prepared PERFORMANCE OF GREASES is listed in table 1.
Embodiment analytical study result is as shown in table 1.
Table 1 embodiment 1～3 gained PERFORMANCE OF GREASES evaluation result
The dropping point of general high temperature resistant lubricating grease is greater than 260 ℃ conventionally, and the PB value of general extreme-pressure lubricating grease is not less than 686N, and PD value is not less than 2452N.And it is known by data in table 1, the dropping point of grease composition of the present invention is greater than 280 ℃, PB value is greater than 686N, PD value is not less than 2452N, therefore employing basicity calcium naphthenate of the present invention is the grease composition that main raw material makes, there is outstanding high thermal resistance and good extreme pressure anti-wear, can meet the lubricating requirement at the larger load equipment of high temperature position.
Claims (10)
1. a high temperature resistant extreme-pressure lubricating grease composition, each constituent mass percentage composition is as follows:
(1) content of the high base number calcium naphthenate that base number is 250～420mgKOH/g is 30～60%;
(2) content of the calcium sulfonate with high base number that base number is 350～420mgKOH/g is 5～20%;
(3) lubricating base oil, surplus.
2. grease composition as claimed in claim 1, the base number that it is characterized in that high base number calcium naphthenate is 280～420mgKOH/g.
3. grease composition as claimed in claim 1, the quality percentage composition that it is characterized in that high base number calcium naphthenate is 30～50%.
4. grease composition as claimed in claim 1, is characterized in that calcium sulfonate with high base number is calcium mahogany sulfonate or calcium alkylbenzenesulfonate.
5. grease composition as claimed in claim 1, the base number that it is characterized in that calcium sulfonate with high base number is 380～420mgKOH/g.
6. grease composition as claimed in claim 1, the quality percentage composition that it is characterized in that calcium sulfonate with high base number is 5～15%.
7. grease composition as claimed in claim 1, is characterized in that lubricating base oil is mineral oil, alkene synthetic oil or its mixture, 100 ℃ of kinematic viscosity 10～60mm
2/ s, open flash point is greater than 240 ℃.
8. the preparation method of grease composition as claimed in claim 1: it is characterized in that 35～65% lubricating base oil of high base number calcium naphthenate, calcium sulfonate with high base number and total lubricating base oil to mix, after stirring, add transforming agent, be warming up to 75～105 ℃, keep 40～120min, material continues to be warming up to 200 ℃ above by water emptying, in temperature-rise period, surplus base oil is added; Material continues to be warming up to 220 ℃～240 ℃, and constant temperature stirs 5～30 minutes, and after material retrogradation, cooling homogenizing obtains required product.
9. preparation method as claimed in claim 8, is characterized in that transforming agent is selected from the mixing of the alkyl benzene sulphonate (ABS) of the lipid acid of C1～C5, fatty alcohol, C8～C15 or two or more material of water.
10. preparation method as claimed in claim 8, is characterized in that transforming agent is selected from two or more mixture of formic acid, acetic acid, propionic acid, ethanol, Virahol, n-propyl alcohol, propyl carbinol, Witco 1298 Soft Acid or water.
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