CN103952215A - High-performance calcium sulfonate complex grease and preparation method thereof - Google Patents
High-performance calcium sulfonate complex grease and preparation method thereof Download PDFInfo
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- CN103952215A CN103952215A CN201410182780.6A CN201410182780A CN103952215A CN 103952215 A CN103952215 A CN 103952215A CN 201410182780 A CN201410182780 A CN 201410182780A CN 103952215 A CN103952215 A CN 103952215A
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Abstract
The invention relates to high-performance calcium sulfonate complex grease and a preparation method thereof. The calcium sulfonate complex grease is prepared from the following raw materials: high-base-number calcium sulfonate, base oil, lauric acid, low-molecular-weight alcohol, high-purity water, boric acid, calcium hydroxide, an antioxidant, and an HL functional additive. The high-performance calcium sulfonate complex grease has the characteristics of being resistant to high temperature, resistant to water, and outstanding in extreme-pressure antiwear property, particularly realizing the uniform distribution of converted calcium carbonate crystal grain, ensuring stable structure, and also solving the problem of surface hardening.
Description
Technical field
The invention belongs to metallurgical technical field of lubricating grease, specifically a kind of high-performance complex calcium sulfonate grease and preparation method thereof.
Background technology
The develop rapidly of the modern industry, more and more higher to the requirement of lubricating grease, the lubricating grease of high-quality multiple-effect is the direction of its development.Composite calcium sulfonate grease lubricant is a class novel lubricating grease, good high temperature performance, mechanical stability, colloid stability, oxidation stability, water resisting property, erosion resistance that it has, excellent rustless property and extreme pressure anti-wear, aspect a lot of, surpassed other high temperature grease as complex lithium grease, composite aluminum base grease and polyurea grease performance.This type of lubricating grease is specially adapted to the lubricated of equipment under steel mill's continuous caster, tandem rolling unit and conditions of similarity, is conducive to simplify lubricating grease kind, and convenience oil management, is called as " high-efficiency lubricating fat ", causes the extensive concern of domestic and international lubricating grease industry.
The patent No. is that the patent of CN102766511A discloses the calcium sulphonate that a kind of complex calcium sulfonate one titanium double composition grease and preparation method thereof this double composition grease is 15～30% by massfraction, 40～60% lubricating base oil, 3～5% carboxylic acid, 5～15% C
12～C
24lipid acid, 5～15% isopropyl titanate, surplus are that high purity water forms.
The patent No., for US4560489 provides a kind of boric acid improved composite calcium sulfonate grease lubricant, comprises calcite calcium carbonate, calcium sulphonate, lime borate and a refreshing C in component
12～C
24aliphatics calcium soap, typical 12-OH stearic acid and boric acid form calcium complex soap.
The patent No. provides a kind of method of preparing the calcite crystal form calcium carbonate solid particulate lubricating grease that contains calcium sulfonate with high base number and disperse with colloid of non newtonian for US5338476.Be included in and in base oil, add calcium sulfonate with high base number, amorphous calcium carbonate and add C
12～C
24the lipid acid of individual carbon atom is done transforming agent.
Above three patents are all to mention the preparation method of grease of calcium sulfonic acid.What patent CN102766511A related generally to calcium sulfonate complex grease and composite titan-based grease becomes fat method and preparation technology, and US5338476 relates to the various aspects of performance that lime borate improves grease of calcium sulfonic acid.
The performance of calcium sulfonate complex grease depends on to a great extent by unformed CaCO in newton's body calcium sulfonate with high base number
3be converted into the transformation of crystal process of the non-newtonian fluid calcium sulphonate of calcite crystal formation.If calcium carbonate containing quantity not sufficient or calcium carbonate wherein from the unformed calcite crystal formation that is not converted into completely, lubricating grease can be partially soft, high-temperature behavior is not good, the sintering load of lubricating grease is on the low side.In addition, after transforming, grain size and the size distribution of the calcium carbonate of calcite crystal formation also can affect the sclerosis of calcium sulfonate complex grease in theory to a great extent from Ostwald slaking, at complex calcium sulfonate grease in storage process, because size distribution is uneven, the trend that can exist particle phase total surface area to reduce, small-particle is consumed gradually, and macroparticle is grown up gradually, thereby has accelerated the surface hardening phenomenon of this type of ravine consistent lubricant.
Summary of the invention
The surface hardening problem that the object of the invention is to solve lubricating grease in prior art, provides a kind of complex calcium sulfonate grease and preparation method thereof.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
A complex calcium sulfonate grease, this complex calcium sulfonate grease is by comprising that following raw material prepares: calcium sulfonate with high base number, base oil, lauric acid, low mass molecule alcohol, high purity water, boric acid, calcium hydroxide, oxidation inhibitor and HL-functional agent.
Preferably, this lubricating grease raw material used and the weight percent of raw material thereof are:
1) calcium sulfonate with high base number: 30～55%;
2) base oil: 20～40%;
3) lauric acid: 5.0～9.0%;
4) low mass molecule alcohol: 1.8～6.0%;
5) high purity water: 6.0～10.0%;
6) boric acid: 0.3～0.6%;
7) calcium hydroxide: 0.6～1.2%;
8) oxidation inhibitor: 0.2～1.0%;
9) HL-functional agent: 0.02～0.05%;
The weight percent sum of above-mentioned raw materials is 100%.
Preferably, this lubricating grease raw material used and the weight percent of raw material thereof are:
1) calcium sulfonate with high base number: 48～54.5%;
2) base oil: 25～30%;
3) lauric acid: 7.0～8.0%;
4) low mass molecule alcohol: 2～3.6%;
5) high purity water: 7.5～8.7%;
6) boric acid: 0.3～0.4%;
7) calcium hydroxide: 0.6～0.75%;
8) oxidation inhibitor: 0.2～0.4%;
9) HL-kinetic energy agent: 0.02～0.03%;
The weight percent sum of above-mentioned raw materials is 100%.
Preferably, described calcium sulfonate with high base number total basicnumber (TBN) is 300～430mgKOH/g.For commercially available prod.
Preferably, described base oil is the mixture of one or more different viscosity grade base oils, and the kinematic viscosity of 40 ℃ is 100～550mm
2/ s.
Preferably, described low mass molecule alcohol is the mixture of one or more alcohol, as one or more the mixture in methyl alcohol, ethanol, propyl carbinol, Virahol.
Preferably, described oxidation inhibitor is the mixture of a kind of in pentanoic, N-phenyl-a-naphthylamine, alkylphenol, di-tertiary butyl methyl phenol or any two kinds.More preferably, described oxidation inhibitor is pentanoic.
Preferably, described HL-functional agent is the anti-water drenching energy while improving calcium sulfonate complex grease high temperature, is commercially available prod.
The present invention also provides the preparation method of described complex calcium sulfonate grease, comprises the following steps:
1) base oil, calcium sulfonate with high base number are placed in to reactor, are heated to 80～90 ℃, and remain on the lasting 40～60min of stirring under this temperature range;
2) lauric acid, low mass molecule alcohol, high purity water are joined to step 1) in the mixture of gained, and at 80～90 ℃, keep continuing stirring reaction to transforming (detecting with infrared spectra) completely, (at this, cross in naked due to material retrogradation, therefore, in order to guarantee to obtain the uniform CaCO of particle diameter
3crystal, needs to stir fully; )
3) after having transformed, by step 2) gained material is warming up to 100～110 ℃, adds successively boric acid and calcium hydroxide, continues stirring reaction 30～40min; Then continue to be warming up to 200～210 ℃, add oxidation inhibitor, and stir 10～20min:
4) by step 3) gained material is cooled to 90～100 ℃ naturally, adds HL-functional agent;
5) the degassed rear finished product of homogenizing.
By implementing above technical scheme, the present invention has following technique effect: the invention provides complex calcium sulfonate grease, the feature with high temperature resistant, water resistant, extreme pressure and antiwear behavior excellence, especially make the calcium carbonate crystal grain after transforming be evenly distributed, make this product structure very stable, solved the surface hardening problem of complex calcium sulfonate grease.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but do not limit protection scope of the present invention.
Embodiment 1
A preparation method for high-performance complex calcium sulfonate grease, comprises the steps:
1) 2409 base oil 150BS, 4239 calcium sulfonate with high base number (TBN is 350mgKOH/g) are placed in to reactor, are heated to 80～90 ℃, and remain on the lasting 40min of stirring under this temperature range;
2) 639 lauric acid, 59 methyl alcohol, 15g ethanol and 709 high purity waters are joined to step 1) in the mixture of gained, and at 80～90 ℃, keep continuing fully to stir, reaction is to transforming (detecting with infrared spectra) completely;
3) after having transformed, by step 2) the tough material of gained is warming up to 100～110 ℃, adds successively 2.8g boric acid and 5.7g calcium hydroxide, continues stirring reaction 30min; Then continue to be warming up to 200～210 ℃, add 2.4g pentanoic as oxidation inhibitor, and stir 10min;
4) by step 3) gained material is cooled to 90～100 ℃ naturally, adds 0.2gHL-functional agent;
5) the degassed rear finished product of homogenizing.
Its performance is listed in to table 1.
Embodiment 2
A high-performance complex calcium sulfonate grease preparation of greases method, comprises the steps:
1) 2409 base oil 150BS, 4239 calcium sulfonate with high base number (TBN is 350mgKOH/g) are placed in to reactor, are heated to 80～90 ℃, and remain on the lasting 40min of stirring under this temperature range;
2) 639 lauric acid, 229 ethanol and 709 high purity waters are joined to step 1) in the mixture of gained, and at 80～90 ℃, keep continuing fully to stir, reaction is to transforming (detecting with infrared spectra) completely;
3) after having transformed, by step 2) gained material is warming up to 100～110 ℃, adds successively 2.8g boric acid and 5.7g calcium hydroxide, continues stirring reaction 30min; Then continue to be warming up to 200～210 ℃, add 2.4g pentanoic as oxidation inhibitor, and stir 10min;
4) by step 3) gained material is cooled to 90～100 ℃ naturally, adds 0.2gHL-functional agent;
5) the degassed rear finished product of homogenizing.
Its performance is listed in to table 1.
Embodiment 3
A high-performance complex calcium sulfonate grease preparation of greases method, comprises the steps:
1) 2409 base oil 150BS, 4239 calcium sulfonate with high base number (TBN is 400mgKOH/g) are placed in to reactor, are heated to 80～90 ℃, and remain on the lasting 40min of stirring under this temperature range;
2) 639 lauric acid, 59 methyl alcohol, 15g ethanol and 709 high purity waters are joined to step 1) in the mixture of gained, and at 80～90 ℃, keep fully continuing to stir, reaction is to transforming (detecting with infrared spectra) completely;
3) after having transformed, by step 2) gained material is warming up to 100～110 ℃, adds successively 2.8g boric acid and 5.7g calcium hydroxide, continues stirring reaction 30min; Then continue to be warming up to 200～210 ℃, add 2.4g pentanoic as oxidation inhibitor, and stir 10min;
4) by step 3) gained material is cooled to 90～100 ℃ naturally, adds 0.2g HL-functional agent;
5) the degassed rear finished product of homogenizing.
Its performance is listed in to table 1.
Embodiment 4
A high-performance complex calcium sulfonate grease preparation of greases method, comprises the steps:
1) 2409 base oil 150BS, 4239 calcium sulfonate with high base number (TBN is 400mgKOH/g) are placed in to reactor, are heated to 80～90 ℃, and remain on the lasting 40min of stirring under this temperature range;
2) 639 lauric acid, 229 ethanol and 709 high purity waters are joined to step 1) in the mixture of gained, and at 80～90 ℃, keep continuing fully to stir, reaction is to transforming (detecting with infrared spectra) completely;
3) after having transformed, by step 2) gained material is warming up to 100～110 ℃, adds successively 2.8g boric acid and 5.7g calcium hydroxide, continues stirring reaction 30min; Then continue out temperature to 200～210 ℃, add 2.4g pentanoic as oxidation inhibitor, and stir 10min;
4) by step 3) gained material is cooled to 90～100 ℃ naturally, adds 0.2g HL-functional agent;
5) the degassed rear finished product of homogenizing.
Its performance is listed in to table 1.
The physical and chemical performance analysis that embodiment 1,2,3,4 prepares gained finished product the results are shown in Table 1.
The physicochemical property of each embodiment lubricating grease of table 1 detects data
The above, be only preferred embodiment of the present invention, not technical scheme of the present invention done to any pro forma restriction.Any simple modification, equivalent variations and modification that every foundation technical spirit of the present invention is done above embodiment, all still belong in the scope of technical scheme of the present invention.
Claims (5)
1. a complex calcium sulfonate grease, is characterized in that: this complex calcium sulfonate grease is by comprising that following raw material prepares: calcium sulfonate with high base number, base oil, lauric acid, low mass molecule alcohol, high purity water, boric acid, calcium hydroxide, oxidation inhibitor and HL-functional agent.
2. a kind of complex calcium sulfonate grease according to claim 1, is characterized in that: the raw material that this lubricating grease is used and the weight percent of raw material thereof are:
1) calcium sulfonate with high base number: 30～55%;
2) base oil: 20～40%;
3) lauric acid: 5.0～9.0%;
4) low mass molecule alcohol: 1.8～6.0%;
5) high purity water: 6.0～10.0%;
6) boric acid: 0.3～0.6%;
7) calcium hydroxide: 0.6～1.2%;
8) oxidation inhibitor: 0.2～1.0%;
9) HL-functional agent: 0.02～0.05%;
The weight percent sum of described raw material is 100%.
3. a kind of complex calcium sulfonate grease according to claim 2, is characterized in that: the raw material that this lubricating grease is used and the weight percent of raw material thereof are:
1) calcium sulfonate with high base number: 48～54.5%;
2) base oil: 25～30%;
3) lauric acid: 7.0～8.0%;
4) low mass molecule alcohol: 2～3.6%;
5) high purity water: 7.5～8.7%;
6) boric acid: 0.3～0.4%;
7) calcium hydroxide: 0.6～0.75%;
8) oxidation inhibitor: 0.2～0.4%;
9) HL-functional agent: 0.02～0.03%;
Weight proportion by subtraction at the tenth of the twelve Earthly Branches sum of described raw material is 100%.
4. according to a kind of complex calcium sulfonate grease described in claim 1-3 any one, it is characterized in that: described calcium sulfonate with high base number total basicnumber is 300～430mgKOH/g.
5. according to a kind of complex calcium sulfonate grease described in claim 1-4 any one, it is characterized in that: described base oil is the mixture of one or more different viscosity grade base oils, and the kinematic viscosity of 40 ℃ is 100～550mm
2/ s.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410182780.6A CN103952215A (en) | 2014-04-24 | 2014-04-24 | High-performance calcium sulfonate complex grease and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410182780.6A CN103952215A (en) | 2014-04-24 | 2014-04-24 | High-performance calcium sulfonate complex grease and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017119999A1 (en) * | 2016-01-07 | 2017-07-13 | Nch Corporation | Method of manufacturing calcium sulfonate greases using delayed addition of non-aqueous converting agents |
| US9976102B2 (en) | 2011-10-31 | 2018-05-22 | Nch Corporation | Composition and method of manufacturing calcium sulfonate greases using alkali metal hydroxide and delayed addition of non-aqueous converting agents |
| US9976101B2 (en) | 2011-10-31 | 2018-05-22 | Nch Corporation | Method of manufacturing calcium sulfonate greases using delayed addition of non-aqueous converting agents |
| US10087388B2 (en) | 2016-05-18 | 2018-10-02 | Nch Corporation | Composition and method of manufacturing calcium sulfonate and calcium magnesium sulfonate greases using a delay after addition of facilitating acid |
| US10087387B2 (en) | 2016-05-18 | 2018-10-02 | Nch Corporation | Composition and method of manufacturing calcium magnesium sulfonate greases |
| US10087391B2 (en) | 2016-05-18 | 2018-10-02 | Nch Corporation | Composition and method of manufacturing calcium magnesium sulfonate greases without a conventional non-aqueous converting agent |
| US10392577B2 (en) | 2016-05-18 | 2019-08-27 | Nch Corporation | Composition and method of manufacturing overbased sulfonate modified lithium carboxylate grease |
| US10519393B2 (en) | 2016-05-18 | 2019-12-31 | Nch Corporation | Composition and method of manufacturing calcium magnesium sulfonate greases |
| CN113736542A (en) * | 2021-08-31 | 2021-12-03 | 江苏澳润新材料有限公司 | Method for improving fineness of high-base-number calcium sulfonate-based lubricating grease |
| US11661563B2 (en) | 2020-02-11 | 2023-05-30 | Nch Corporation | Composition and method of manufacturing and using extremely rheopectic sulfonate-based greases |
-
2014
- 2014-04-24 CN CN201410182780.6A patent/CN103952215A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9976102B2 (en) | 2011-10-31 | 2018-05-22 | Nch Corporation | Composition and method of manufacturing calcium sulfonate greases using alkali metal hydroxide and delayed addition of non-aqueous converting agents |
| US9976101B2 (en) | 2011-10-31 | 2018-05-22 | Nch Corporation | Method of manufacturing calcium sulfonate greases using delayed addition of non-aqueous converting agents |
| WO2017119999A1 (en) * | 2016-01-07 | 2017-07-13 | Nch Corporation | Method of manufacturing calcium sulfonate greases using delayed addition of non-aqueous converting agents |
| US10087388B2 (en) | 2016-05-18 | 2018-10-02 | Nch Corporation | Composition and method of manufacturing calcium sulfonate and calcium magnesium sulfonate greases using a delay after addition of facilitating acid |
| US10087387B2 (en) | 2016-05-18 | 2018-10-02 | Nch Corporation | Composition and method of manufacturing calcium magnesium sulfonate greases |
| US10087391B2 (en) | 2016-05-18 | 2018-10-02 | Nch Corporation | Composition and method of manufacturing calcium magnesium sulfonate greases without a conventional non-aqueous converting agent |
| US10392577B2 (en) | 2016-05-18 | 2019-08-27 | Nch Corporation | Composition and method of manufacturing overbased sulfonate modified lithium carboxylate grease |
| US10519393B2 (en) | 2016-05-18 | 2019-12-31 | Nch Corporation | Composition and method of manufacturing calcium magnesium sulfonate greases |
| US11168277B2 (en) | 2016-05-18 | 2021-11-09 | Nch Corporation | Composition and method of manufacturing calcium magnesium sulfonate greases |
| US12031100B2 (en) | 2016-05-18 | 2024-07-09 | Nch Corporation | Composition and method of manufacturing calcium magnesium sulfonate greases |
| US11661563B2 (en) | 2020-02-11 | 2023-05-30 | Nch Corporation | Composition and method of manufacturing and using extremely rheopectic sulfonate-based greases |
| CN113736542A (en) * | 2021-08-31 | 2021-12-03 | 江苏澳润新材料有限公司 | Method for improving fineness of high-base-number calcium sulfonate-based lubricating grease |
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Application publication date: 20140730 |