CN115772435B - Composite calcium type automobile hub bearing lubricating grease composition and preparation method thereof - Google Patents
Composite calcium type automobile hub bearing lubricating grease composition and preparation method thereof Download PDFInfo
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- CN115772435B CN115772435B CN202211468670.7A CN202211468670A CN115772435B CN 115772435 B CN115772435 B CN 115772435B CN 202211468670 A CN202211468670 A CN 202211468670A CN 115772435 B CN115772435 B CN 115772435B
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- 239000004519 grease Substances 0.000 title claims abstract description 62
- 230000001050 lubricating effect Effects 0.000 title claims abstract description 51
- 239000002131 composite material Substances 0.000 title claims abstract description 44
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000011575 calcium Substances 0.000 title claims abstract description 43
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 43
- 239000000203 mixture Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title abstract description 17
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 32
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 30
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims abstract description 24
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims abstract description 24
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 18
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 18
- 239000005711 Benzoic acid Substances 0.000 claims abstract description 12
- 235000010233 benzoic acid Nutrition 0.000 claims abstract description 12
- 235000019260 propionic acid Nutrition 0.000 claims abstract description 12
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims abstract description 12
- 229940114072 12-hydroxystearic acid Drugs 0.000 claims abstract description 10
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 9
- 150000001336 alkenes Chemical class 0.000 claims abstract description 6
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000008117 stearic acid Substances 0.000 claims abstract description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 11
- 239000000725 suspension Substances 0.000 claims description 11
- 239000012964 benzotriazole Substances 0.000 claims description 8
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 238000010791 quenching Methods 0.000 claims description 7
- 230000000171 quenching effect Effects 0.000 claims description 7
- 238000005096 rolling process Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000002199 base oil Substances 0.000 abstract description 15
- 239000002562 thickening agent Substances 0.000 abstract description 14
- 150000007524 organic acids Chemical class 0.000 abstract description 12
- 239000003795 chemical substances by application Substances 0.000 abstract description 8
- 230000000996 additive effect Effects 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000000654 additive Substances 0.000 abstract description 6
- DKVNPHBNOWQYFE-UHFFFAOYSA-N carbamodithioic acid Chemical compound NC(S)=S DKVNPHBNOWQYFE-UHFFFAOYSA-N 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 13
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 12
- 239000002253 acid Substances 0.000 description 8
- 238000003860 storage Methods 0.000 description 8
- 239000003513 alkali Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 239000007795 chemical reaction product Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 229910052744 lithium Inorganic materials 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- CXZIVLHEAFSOQK-UHFFFAOYSA-K bismuth;tricarbamodithioate Chemical compound [Bi+3].NC([S-])=S.NC([S-])=S.NC([S-])=S CXZIVLHEAFSOQK-UHFFFAOYSA-K 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- -1 calcium phenylborate-calcium phosphate Chemical compound 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 239000013556 antirust agent Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 235000015278 beef Nutrition 0.000 description 1
- 125000003354 benzotriazolyl group Chemical group N1N=NC2=C1C=CC=C2* 0.000 description 1
- 235000014121 butter Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010696 ester oil Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- UFWIBTONFRDIAS-UHFFFAOYSA-N naphthalene-acid Natural products C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/80—Technologies aiming to reduce greenhouse gasses emissions common to all road transportation technologies
- Y02T10/86—Optimisation of rolling resistance, e.g. weight reduction
Landscapes
- Lubricants (AREA)
Abstract
The invention belongs to the technical field of lubricating grease, and provides a composite calcium type automobile hub bearing lubricating grease composition and a preparation method thereof, wherein the composite comprises base oil, a thickening agent and an additive, the additive comprises an extreme pressure antiwear agent, and raw materials for preparing the thickening agent comprise calcium hydroxide and potassium hydroxide in a weight ratio of 10-8:0-2, and a long-chain organic acid composed of propionic acid, benzoic acid and terephthalic acid in a weight ratio of 0-6:0-2:10-4, and a long-chain organic acid composed of 12-hydroxystearic acid and stearic acid in a weight ratio of 10-8:0-2; the extreme pressure antiwear agent is more than one of ZDDP, sulfurized olefin, bismuth naphthenate and dialkyl dithiocarbamic acid bismuth. According to the invention, the problem of surface hardening of the automobile hub bearing lubricating grease is effectively solved by selecting specific raw materials, and the use temperature range of the prepared lubricating grease is as follows: the temperature is between 30 ℃ below zero and 150 ℃, the performances are excellent, the bearing is suitable for automobile hub bearings.
Description
Technical Field
The invention relates to the technical field of lubricating grease, in particular to a composite calcium type automobile hub bearing lubricating grease composition and a preparation method thereof.
Background
The automobile hub bearing has higher rotating speed, certain impact load, especially overload phenomenon, and the sealing structure is common, so that dust, water and external impurities can pollute the automobile, and the automobile has wide running field. Therefore, the automotive hub bearing grease is required to have good temperature resistance, lubricity, water resistance, wear resistance, rust resistance and adhesion, and a wide use temperature range.
The composite lithium grease is multifunctional grease, extreme pressure composite lithium with higher base oil viscosity is very suitable for lubricating automobile hub bearings, especially commercial automobile hubs, and currently, the primary assembly and the host market are basically composite lithium type products, so that the application effect is good. In recent years, the price of lithium hydroxide is increased by about 10 times, and the lithium hydroxide brings great cost pressure to the grease for the automobile hub bearing. The traditional composite calcium-based lubricating grease is composite calcium soap formed by long-chain organic acid and acetic acid, has good temperature resistance, extreme pressure property and lubricity, but is seriously hardened in the storage process, so that the popularization and the application of the composite calcium-based lubricating grease are limited. If the composite calcium-based lubricating grease can solve the hardening problem in storage, the composite calcium-based lubricating grease has obvious cost advantages due to good high-temperature property, extreme pressure property and lubricity, and has popularization prospect in the aspect of automobile hub bearing lubricating grease. For this reason, attempts have been made to overcome some of the drawbacks of complex calcium-based greases by improving them so that they can be adapted to the lubrication of hubs, as in patent application CN111718778A by introducing a calcium phenylborate-calcium phosphate component to provide the hub bearing grease with anti-friction wear and anti-oxidation capabilities, while improving the problem of storage hardening of the complex calcium-based greases, but the manufacturing process is complex.
In view of this, the present invention has been proposed.
Disclosure of Invention
The invention provides a composite calcium type automobile hub bearing lubricating grease composition and a preparation method thereof, wherein the composite calcium type automobile hub bearing lubricating grease composition which has small surface hardening after long-time storage, simple process, stability and feasibility and lower preparation cost is prepared by selecting raw materials and designing a formula, so that the defects of high cost, complex preparation method and the like of lubricating grease suitable for automobile hub bearings in the prior art are overcome.
The invention provides a composite calcium type automobile hub bearing lubricating grease composition, which comprises base oil, a thickening agent and an additive, wherein the additive comprises an extreme pressure antiwear agent, and the extreme pressure antiwear agent is more than one of ZDDP, sulfurized olefin, bismuth naphthenate and dialkyl bismuth dithiocarbamate;
the raw materials for preparing the thickener comprise calcium hydroxide and potassium hydroxide with the weight ratio of 10-8:0-2, and small molecular organic acid composed of propionic acid, benzoic acid and terephthalic acid with the weight ratio of 0-6:0-2:10-3, and long chain organic acid composed of 12-hydroxystearic acid and stearic acid with the weight ratio of 10-8:0-2;
the weight ratio of the long-chain organic acid to the small-molecule organic acid is 162:54-81; the ratio of the total mass of the long-chain organic acid to the total mass of the calcium hydroxide and the potassium hydroxide is 162:68-80.
In order to obtain excellent comprehensive performance, particularly, the prepared lubricating grease can improve the surface hardening problem while the service temperature and extreme pressure performance meet the requirements of automobile hub bearings, the special extreme pressure antiwear agent and thickening agent are selected, the purposes are achieved through a special formula design, and the selected raw materials are easy to obtain, lower in cost and higher in technical value. Preferably, when the extreme pressure antiwear agent used in the present invention is mixed with the above substances in a certain ratio, the performance of the prepared grease is more excellent than when a single substance is used as the extreme pressure antiwear agent.
Regarding the alkali used for preparing the thickener, the alkali substances such as calcium hydroxide and the like commonly used in the prior art participate in the reaction to form the thickener, and the invention can more obviously improve the storage stability of the lubricating grease by mixing a small amount of potassium hydroxide into the calcium hydroxide, for example, when the weight ratio of the calcium hydroxide to the potassium hydroxide is 9:1, the variation value of the surface hardness is the smallest.
In addition, the selection of the small molecular acid is also very critical to the surface hardening of the lubricating grease during storage, which is not only related to the type of the small molecular acid, but also has larger influence on the performance due to the type of the small molecular acid and the proportion of various acids, for example, when the weight ratio of propionic acid, benzoic acid and terephthalic acid is 1-3:0-1:9-6, the obtained lubricating grease has smaller variation of the cone penetration value after being stored for 6 months;
preferably, when the long-chain organic acid is 12-hydroxystearic acid, the prepared composite calcium type automobile hub bearing grease composition has better stability.
The small molecular organic acid composed of propionic acid, benzoic acid and terephthalic acid with the weight ratio of 0-6:0-2:10-3 can be understood as follows: when the small molecular organic acid contains propionic acid, benzoic acid and terephthalic acid at the same time, the mass ratio of the propionic acid to the terephthalic acid in the small molecular acid is 0-6:10-3, the mass ratio of the benzoic acid to the terephthalic acid is 0-2:10-3, and the mass ratio of the propionic acid to the benzoic acid is 0-6:0-2; when the small molecular acid only contains propionic acid and terephthalic acid, the mass ratio of the propionic acid to the terephthalic acid in the small molecular acid is 0-6:10-3; when the small molecular acid only contains benzoic acid and terephthalic acid, the mass ratio of the benzoic acid to the terephthalic acid is 0-2:10-3.
According to the composite calcium type automobile hub bearing lubricating grease composition provided by the invention, the addition amount of the extreme pressure antiwear agent is 1.5-5.0%, preferably 2.5-5.0%, more preferably 3.0-4.0% of the total mass of the base oil and the thickening agent.
According to the composite calcium type automobile hub bearing lubricating grease composition provided by the invention, the weight ratio of the base oil to the thickening agent is 75-85:15-25.
The composite calcium type automobile hub bearing lubricating grease composition provided by the invention further comprises a high polymer accounting for 0.5-3.0% of the total mass of base oil and thickener, wherein the high polymer consists of PIB, OCP or powder rubber;
preferably, the additive further comprises a high molecular polymer accounting for 0.8-2.5% of the total mass of the base oil and the thickening agent.
The composite calcium type automobile hub bearing lubricating grease composition provided by the invention further comprises an antioxidant accounting for 0.7-1.2% of the total mass of base oil and thickener, preferably 1.0%, wherein the antioxidant is diisodioctyl diphenylamine.
The composite calcium type automobile hub bearing lubricating grease composition provided by the invention further comprises an antirust agent accounting for 0.06-0.08% of the total mass of the base oil and the thickening agent, preferably 0.08%, wherein the antirust agent is benzotriazole.
The composite calcium type automobile hub bearing lubricating grease composition provided by the invention has the advantages that the base oil is mineral oilAnd/or synthetic oils; the viscosity of the base oil at 40 ℃ is 150-230 mm 2 And/s. The synthetic oil is an ester oil, an alkyl naphthalene or a polyolefin oil.
The invention also provides a preparation method of the composite calcium type automobile hub bearing lubricating grease composition, which comprises the following steps:
mixing a part of base oil and long-chain organic acid, adding a first part of alkali liquor at 80-90 ℃ to react for 40-65 min at 100-110 ℃ to obtain a first reaction product;
heating the first reaction product to 110-120 ℃, adding small molecular organic acid to react for 15-25 min, and then adding a second part of alkali liquor to react for 40-60 min to obtain a second reaction product;
heating the second reaction product to 210-230 ℃ and keeping the temperature for 3-7 min, adding the rest base oil, uniformly mixing, and naturally cooling to 80-110 ℃ to obtain a third reaction product;
and adding the additive into a third reaction product, cooling to 70-80 ℃, and then performing oil rolling or homogenizing to obtain the composite calcium type automobile hub bearing lubricating grease composition.
The oil rolling can be performed by a three-roller machine.
The homogenization can be performed by a homogenizer.
According to the preparation method of the composite calcium type automobile hub bearing lubricating grease composition provided by the invention, the weight ratio of the calcium hydroxide in the first part of alkali liquor to the second part of alkali liquor is 30:34-42;
and/or, the part of the base oil accounts for 70-80% of the total mass of the base oil.
According to the preparation method of the composite calcium type automobile hub bearing lubricating grease composition provided by the invention, potassium hydroxide is fully added into the first part of alkali liquor; i.e. the potassium hydroxide is added in its entirety at the first addition of the lye.
The composite calcium type automobile hub bearing lubricating grease composition prepared by the invention is prepared by selecting raw material types in a formula, examining the addition amount, particularly the formula of a thickening agent, so that the cone penetration change value of the 200L packaged composite calcium type automobile hub bearing lubricating grease composition obtained by mass production of the composite calcium type automobile hub bearing lubricating grease composition is within 10 units after outdoor and outdoor open-air storage time in winter to summer is up to 6 months, and no obvious hardening phenomenon exists on the surface and below. The application temperature range of the composite calcium type automobile hub bearing lubricating grease composition provided by the invention is as follows: the lubricating oil is excellent in comprehensive performance at the temperature of 30 ℃ below zero to 150 ℃ below zero, and is suitable for lubricating automobile hub bearings.
The preparation method of the composite calcium type automobile hub bearing lubricating grease composition provided by the invention is further combined with the control of technological parameters in the preparation process on the basis of formula design, and effectively solves the problem of hardening of composite calcium type lubricating grease. The method has the advantages of easily available raw materials, simple process, low cost, no special requirements on production equipment and capability of meeting the production requirement of the normal pressure kettle.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The specific techniques or conditions are not identified in the examples and are described in the literature in this field or are carried out in accordance with the product specifications. The reagents or equipment used were conventional products available for purchase by regular vendors without the manufacturer's attention.
MVI500, 150BS, beef tallow are commercial products, wherein the MVI500, 150BS have a viscosity of 85mm at 40 DEG C 2 /s、320mm 2 /s。
The ZDDP, PIB, OCP and powdered rubber are commercial products, and are purchased from the Lubo additive Co., ltd.
Example 1
A preparation method of a composite calcium type automobile hub bearing lubricating grease composition comprises the following steps: 400g of MVI500, 200g of 150BS, 129.6g of 12-hydroxystearic acid and 32.4g of stearic acid are added into a reaction kettle, stirring is started, heating is carried out to 80 ℃, a suspension formed by 30g of calcium hydroxide, 7.2g of potassium hydroxide and 150g of water which are prepared in advance is added into the reaction kettle, and stirring is carried out for 40 minutes at 110 ℃; heating to 110 ℃, adding 19.4g of terephthalic acid and 12.9g of benzoic acid as solids, and then adding 32.4g of propionic acid; after dispersing and stirring for 20 minutes, dropwise adding a suspension formed by 34.6g of calcium hydroxide and 180g of water prepared in advance, continuing stirring for 40 minutes, heating to 220 ℃, and keeping the temperature for 5 minutes; 200g of 150BS is added as quenching oil, the temperature is reduced to 110 ℃, 10.3g of diisodioctyl diphenylamine, 0.8g of benzotriazole, 15.4g of dialkyl bismuth dithiocarbamate and 15.4g ZDDP,30.8g PIB are added; naturally cooling to 70 ℃, and rolling the materials by a three-roller machine to obtain the composite calcium type automobile hub bearing lubricating grease composition.
Example 2
A preparation method of a composite calcium type automobile hub bearing lubricating grease composition comprises the following steps: adding 560g of MVI500, 145.8g of 12-hydroxystearic acid and 16.2g of stearic acid into a reaction kettle, starting stirring, heating to 90 ℃, adding a suspension formed by 30g of calcium hydroxide prepared in advance and 150g of water into the reaction kettle, and stirring for 60 minutes at 100 ℃; heating to 120 ℃, adding 18.9g of terephthalic acid and 2.7g of benzoic acid as solids, and then adding 32.4g of propionic acid; after dispersing and stirring for 20 minutes, dropwise adding a suspension formed by 38.2g of calcium hydroxide and 200g of water, stirring for 60 minutes, heating to 220 ℃, and keeping the temperature for 5 minutes; 240g 150BS is added as quenching oil, the temperature is reduced to 80 ℃, 10.3g diisodioctyl diphenylamine, 0.8g benzotriazole, 10.2g vulcanized olefin, 20.3g ZDDP,15.2g bismuth naphthenate and 5.1g OCP are added; naturally cooling to 70 ℃, and rolling the materials by a three-roller machine to obtain the composite calcium type automobile hub bearing lubricating grease composition.
Example 3
A preparation method of a composite calcium type automobile hub bearing lubricating grease composition comprises the following steps: 500Kg MVI500, 300Kg 150BS and 162Kg 12-hydroxystearic acid are added into a reaction kettle, stirring is started, heating is carried out to 85 ℃, suspension formed by 30Kg of calcium hydroxide, 8Kg of potassium hydroxide and 150Kg of water which are prepared in advance is added into the reaction kettle, and stirring is carried out for 50 minutes at 105 ℃; heating to 115 ℃, adding 81kg of solid terephthalic acid, dispersing and stirring for 20 minutes, then starting to dropwise add a suspension formed by 42kg of calcium hydroxide and 200kg of water, continuing stirring for 50 minutes, heating to 220 ℃, and keeping the temperature for 5 minutes; 200Kg MVI500 is added as quenching oil, the temperature is reduced to 100 ℃, 10.3Kg of diisodioctyl diphenylamine, 0.8Kg of benzotriazole, 12.4Kg of bismuth naphthenate and 12.4Kg ZDDP,18.6Kg Kg of bismuth dialkyldithiocarbamate and 18.6Kg of powdered rubber are added; naturally cooling to 75 ℃, and homogenizing the materials by a homogenizer to obtain the composite calcium type automobile hub bearing lubricating grease composition.
Comparative example 1
A preparation method of the lubricating grease composition comprises the following steps: 2000g MVI500, 180g butter, 180g 12-hydroxystearic acid are added into a reaction kettle, stirring is started, heating is carried out to 85 ℃, and stirring is carried out for 30 minutes at the temperature; slowly adding 90g of acetic acid into a reaction kettle, stirring for 20 minutes, adding a suspension formed by 165g of calcium hydroxide and 500g of water, reacting for 2 hours at 100 ℃, slowly heating to 150 ℃, adding 1000g of heating oil 150BS, continuously heating to 220 ℃, and keeping the temperature for 5 minutes; 500g of 150BS is added as quenching oil, the temperature is reduced to 165 ℃, 500g of 150BS cooling oil is added, natural cooling is carried out to 80 ℃, 44.5g of diisodioctyl diphenylamine, 35.6g of benzotriazole 22.2g of sulfurized olefin, 66.8g of ZDDP,66.8g of dialkyl bismuth dithiocarbamate and 66.8g of powdered rubber are added, and the material is rolled by a three-roller machine to obtain the lubricating grease composition.
Comparative example 2
A preparation method of the lubricating grease composition comprises the following steps: adding 1300g of MVI500, 700g of 150BS, 250g of 12-hydroxystearic acid and 125g of azelaic acid into a reaction kettle, starting stirring, heating to 85 ℃, adding a solution formed by 40g of lithium hydroxide prepared in advance and 200g of water, reacting for 2 hours at 100 ℃, slowly heating to 110 ℃, dropwise adding a solution formed by the rest 42.5g of lithium hydroxide prepared in advance and 200g of water for 1 hour, slowly heating to drain water, and continuously heating to 220 ℃ and keeping the temperature constant for 5 minutes; 300g of 150BS is added as quenching oil, the temperature is reduced to 165 ℃, 300g of 150BS cooling oil is added, natural cooling is carried out to 80 ℃, 44.5g of diisodioctyl diphenylamine, 35.6g of benzotriazole, 14.9g of vulcanized olefin, 44.6g of ZDDP,44.6g of dialkyl bismuth dithiocarbamate and 44.6g of powdered rubber are added, and the materials are rolled by a three-roller machine to obtain the lubricating grease composition.
The greases obtained in examples 1 to 3 and comparative examples 1 to 2 were tested and the test results were as follows:
TABLE 1
As can be seen from Table 1, the composite calcium type automobile hub bearing grease composition prepared by the method of examples 1-3 of the invention is equivalent to the traditional composite calcium type grease and composite lithium type grease represented by comparative examples 1-2 in the aspects of lubricity, high temperature resistance, water resistance, corrosion resistance and the like. The complex calcium type automobile hub bearing grease compositions prepared in examples 1 to 3 showed a small change in penetration after 6 months of storage under outdoor and outdoor conditions from winter to summer, compared with the complex calcium type grease of comparative example 1, and were significantly improved in terms of hardening, and also improved in terms of extreme pressure performance, compared with the complex lithium type grease of comparative example 2.
Finally, it should be noted that the above embodiments are only for illustrating the technical scheme of the present invention, and are not limiting; while the invention has been described in detail with reference to the foregoing embodiments, it will be appreciated by those skilled in the art that variations may be made in the techniques described in the foregoing embodiments, or equivalents may be substituted for elements thereof; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (2)
1. A composite calcium type automobile hub bearing lubricating grease composition is characterized in that 560g of MVI500, 145.8g of 12-hydroxystearic acid and 16.2g of stearic acid are added into a reaction kettle, stirring is started, heating is carried out to 90 ℃, a suspension formed by 30g of calcium hydroxide and 150g of water, which is prepared in advance, is added into the reaction kettle, and stirring is carried out for 60 minutes at 100 ℃; heating to 120 ℃, adding 18.9g of terephthalic acid and 2.7g of benzoic acid as solids, and then adding 32.4g of propionic acid; after dispersing and stirring for 20 minutes, dropwise adding a suspension formed by 38.2g of calcium hydroxide and 200g of water, stirring for 60 minutes, heating to 220 ℃, and keeping the temperature for 5 minutes; 240g 150BS is added as quenching oil, the temperature is reduced to 80 ℃, 10.3g diisodioctyl diphenylamine, 0.8g benzotriazole, 10.2g vulcanized olefin, 20.3g ZDDP,15.2g bismuth naphthenate and 5.1g OCP are added; naturally cooling to 70 ℃, and rolling the materials by a three-roller machine to obtain the product.
2. A composite calcium type automobile hub bearing lubricating grease composition is characterized in that 500Kg of MVI500, 300Kg of 150BS and 162Kg of 12-hydroxystearic acid are added into a reaction kettle, stirring is started, heating is carried out to 85 ℃, suspension formed by 30Kg of calcium hydroxide, 8Kg of potassium hydroxide and 150Kg of water which are prepared in advance is added into the reaction kettle, and stirring is carried out for 50 minutes at 105 ℃; heating to 115 ℃, adding 81kg of solid terephthalic acid, dispersing and stirring for 20 minutes, then starting to dropwise add a suspension formed by 42kg of calcium hydroxide and 200kg of water, continuing stirring for 50 minutes, heating to 220 ℃, and keeping the temperature for 5 minutes; 200Kg MVI500 is added as quenching oil, the temperature is reduced to 100 ℃, 10.3Kg of diisodioctyl diphenylamine, 0.8Kg of benzotriazole, 12.4Kg of bismuth naphthenate and 12.4Kg ZDDP,18.6Kg Kg of bismuth dialkyldithiocarbamate and 18.6Kg of powdered rubber are added; naturally cooling to 75 ℃, and homogenizing the materials by a homogenizer.
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