CN111334357A - Mineral oil lithium-based lubricating grease and preparation process thereof - Google Patents
Mineral oil lithium-based lubricating grease and preparation process thereof Download PDFInfo
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- CN111334357A CN111334357A CN202010289558.1A CN202010289558A CN111334357A CN 111334357 A CN111334357 A CN 111334357A CN 202010289558 A CN202010289558 A CN 202010289558A CN 111334357 A CN111334357 A CN 111334357A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M143/00—Lubricating compositions characterised by the additive being a macromolecular hydrocarbon or such hydrocarbon modified by oxidation
- C10M143/10—Lubricating compositions characterised by the additive being a macromolecular hydrocarbon or such hydrocarbon modified by oxidation containing aromatic monomer, e.g. styrene
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/102—Aliphatic fractions
- C10M2203/1025—Aliphatic fractions used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/022—Ethene
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/024—Propene
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/04—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing aromatic monomers, e.g. styrene
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/02—Hydroxy compounds
- C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
- C10M2207/026—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
- C10M2207/1265—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic used as thickening agent
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/127—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids polycarboxylic
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
- C10M2207/1285—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof used as thickening agents
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
- C10M2215/064—Di- and triaryl amines
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/22—Heterocyclic nitrogen compounds
- C10M2215/223—Five-membered rings containing nitrogen and carbon only
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
Abstract
The invention relates to a structure-enhanced mineral oil lithium-based lubricating grease and a preparation method thereof; the lubricating grease comprises 85-92% of base oil, 8-14% of thickening agent, 0.1-0.5% of structure improver, 0.3-0.5% of antioxidant and 0.1-0.3% of antirust agent; adding part of mineral oil into a reaction kettle, adding fatty acid and a structure improver, heating to 60 ℃, adding lithium hydroxide monohydrate and water, heating to 150-160 ℃ in a sealed manner, and carrying out heat preservation reaction for 0.5-1 hour; after saponification, raising the temperature to 170-180 ℃, starting pressure relief and water discharge steam, raising the temperature to 200-215 ℃, then entering a quenching mixer together with part of base oil for cooling, and controlling the cooling temperature at 170-190 ℃; adding the rest base oil, circularly shearing, cooling to 110-130 ℃, and homogenizing by using a high-pressure homogenizer; and cooling to 70-90 ℃, adding an antioxidant and an antirust agent, adjusting the consistency, and degassing to obtain a lubricating grease finished product. The lubricating grease produced by the invention has excellent structural stability, shear resistance and adhesiveness, and can effectively prolong the lubricating life.
Description
Technical Field
The invention relates to the technical field of preparation of lithium-based lubricating grease, and particularly relates to mineral oil lithium-based lubricating grease and a preparation process thereof.
Background
Lithium grease is the most widely used grease at present, and accounts for more than 60% of the total amount of grease in China, and becomes a representative of the variety composition and technical level of grease in China. In addition to the increase in number and share, the development of lithium-based grease varieties is also very rapid. There are now a series of lithium grease products prepared from 12-hydroxystearic acid, stearic acid and lithium soap of hydrogenated castor oil; lithium-based grease products having mineral oil and various synthetic oils as base oils; the lubricating grease contains extreme pressure antiwear and antirust lithium base grease products. Wherein the mineral oil lithium-based lubricating grease accounts for more than 90 percent, and is widely applied to the lubrication of automobile hubs, chassis, motor bearings, various mechanical equipment and transmission parts.
With the increasing attention of the country to energy conservation and environmental protection, the problems of easy thinning and loss, insufficient lubrication life and the like are exposed in the actual use of the mineral oil lithium-based lubricating grease, so that the environmental pollution and the resource waste are caused. At present, the annual consumption of Chinese lubricating grease accounts for about one third of the total amount of the lubricating grease in the world, the consumption is large, the quality of the lubricating grease is improved, and the reduction of unit GDP lubricating grease consumption is the responsibility of lubricating grease workers.
At present, Chinese patent with publication number CN102433203A discloses a lithium-based lubricating grease composition and a preparation method thereof, wherein the lithium-based lubricating grease composition comprises 85-96% of base oil; 3-14% of a thickening agent; 0.5 percent of antioxidant; 0.5 percent of tackifier, wherein the tackifier is polyisobutylene, polymethacrylate or ethylene-propylene copolymer.
Chinese patent No. CN103468357B discloses a water-resistant extreme pressure lithium grease and a preparation method thereof, which comprises the following components: 70-90% of base oil, 9-15% of fatty acid, 1-2% of lithium hydroxide, 0.3-0.7% of calcium hydroxide powder, 0.1-0.5% of antioxidant, 0.3-1.5% of antirust agent, 2-5% of extreme pressure agent and 2-5% of tackifier, wherein the tackifier is at least one of polyisobutylene and ethylene propylene copolymer.
Chinese patent No. CN100358987C discloses a high extreme pressure lithium-based grease, which comprises high viscosity mineral oil: 78-81 parts; fatty acid: 7-10 parts; lithium hydroxide: 0.9-1.5 parts; calcium hydroxide: 0.3-0.5 part; antioxidant: 0.5-1.5 parts; extreme pressure agent: 3-6 parts; an oiliness agent: 2-5 parts; tackifier: 2-5 parts of a tackifier, wherein the tackifier is random polypropylene.
The prior art disclosed above all uses a method of adding a tackifier to the grease, and common tackifiers are polyisobutylene, polymethacrylate, ethylene-propylene copolymer, and polypropylene. The polymer serving as the tackifier has good compatibility with base oil, is added at the later stage of the production of the lubricating grease and dissolved in the base oil, improves the viscosity of the base oil, but cannot form a three-dimensional network structure, cannot effectively improve the strength of a fiber structure of the lithium-based lubricating grease, the fiber structure of the lubricating grease is easily damaged under a high-shear working condition or when the lubricating grease is contacted with polar substances (such as water and organic solvents), and the lubricating grease is still easy to thin and run off.
Disclosure of Invention
The invention aims to provide a mineral oil lithium-based lubricating grease and a preparation process thereof. Compared with traditional polyisobutylene, polymethacrylate, ethylene-propylene copolymer and polypropylene, SEEPS has excellent high tensile strength and shear stability, polymer molecules are not easy to shear, and meanwhile, the SEEPS has excellent high-temperature stability and weather resistance.
The technical purpose of the invention is realized by the following technical scheme:
a lithium mineral oil grease comprising the components in weight percent: 85-92% of base oil, 8-14% of thickening agent, 0.1-0.5% of structure improver, 0.3-0.5% of antioxidant and 0.1-0.3% of antirust agent.
Further, the viscosity of the base oil is 8.5-16 mm at 100 DEG C2One or more of paraffin-based mineral oil, intermediate-based mineral oil or naphthenic-based mineral oil in the second step.
Further, the thickening agent is fatty acid lithium soap, the fatty acid lithium soap is a product obtained by saponification of fatty acid and lithium hydroxide, and the fatty acid is a mixture of 12-hydroxystearic acid and stearic acid.
Furthermore, the stearic acid accounts for 10-30% of the weight of the fatty acid.
Further, the structure improver is a styrene-ethylene-propylene-styrene block copolymer, and the number average molecular weight of the block copolymer is 15 to 25 ten thousand.
Further, the antioxidant is an amine antioxidant or a phenol antioxidant.
Further, the antirust agent is one of benzotriazole, barium dinonylnaphthalene sulfonate and dodecenylsuccinic acid.
A preparation process of mineral oil lithium-based lubricating grease comprises the following steps:
s1: adding 30-50% of all base oil, fatty acid and a structure improver into a reaction kettle, fully mixing, heating and raising the temperature;
s2: after the temperature in the kettle rises to 60 ℃, adding lithium hydroxide monohydrate and water with the weight 1-2 times that of the lithium hydroxide monohydrate into the reaction kettle, and then starting to raise the temperature for saponification reaction;
s3: when the temperature is increased to 150 ℃ and 160 ℃, the reaction is carried out for 0.5 to 1 hour under the condition of heat preservation;
s4: continuously heating to 170-180 ℃, and relieving pressure of the reaction kettle to discharge water vapor, wherein the highest refining temperature is 200-215 ℃;
s5: after refining, quickly cooling the high-temperature materials and 15-30% of base oil in the kettle through a quenching mixer, controlling the temperature to be 170-190 ℃ after quenching, and then transferring the quenched materials into a cooling kettle;
s6: continuously cooling the materials into grease, adding the residual base oil, performing circular shearing, and homogenizing by using a high-pressure homogenizer when the temperature is reduced to 110-130 ℃;
s7: and (3) cooling the material to 70-90 ℃, adding an antioxidant and an antirust agent, regulating and degassing to obtain a finished lubricating grease product.
Further, in step S4, the maximum refining temperature of the autoclave after the pressure release is controlled to be 200 to 215 ℃.
In conclusion, the invention has the following beneficial effects:
1. the styrene-ethylene-propylene-styrene block copolymer (SEEPS) is used as an improver of a lithium soap fiber structure of fatty acid, so that the structural strength of the lithium soap fiber is improved, compared with the traditional polyisobutylene, polymethacrylate, ethylene-propylene copolymer and polypropylene, the SEEPS has excellent high tensile strength and shear stability, polymer molecules are not easy to shear, and meanwhile, the SEEPS has excellent high-temperature stability and weather resistance, and due to the particularity of the molecular structure, the SEEPS is sensitive to temperature in oil, can be separated out from lubricating oil to form a three-dimensional network structure along with the reduction of temperature, so that the stability of the lubricating grease structure is enhanced;
2. the SEEPS is added in the feeding stage, the fatty acid lithium soap is melted in the base oil in the high-temperature refining stage, the SEEPS polymer molecule coil is also stretched out from a bulk shape, and then the SEEPS polymer molecules are separated out from the base oil in the forming process of the fatty acid lithium soap fiber structure through rapid cooling of a rapid cooling mixer to form a three-dimensional network structure, and the network structure is interwoven with the three-dimensional network structure of the fatty acid lithium soap fiber, so that the stability of the lubricating grease fiber structure is enhanced, and the shear resistance of the lubricating grease is obviously improved. And in practical application, due to the high tensile strength of the SEEPS polymer and the strong adhesive force between the SEEPS polymer and the metal surface, the loss of the lubricating grease in the using process is obviously reduced. The service life of the lubricating grease prepared by the method is obviously prolonged, and the grease replacement period is prolonged from 1.5-3 kilometres to 6 kilometres when the lubricating grease is applied to a commercial wheel hub bearing;
3. due to the high tensile strength of the SEEPS polymer and the strong adhesive force between the SEEPS polymer and the metal surface, the loss of the lubricating grease in the using process is obviously reduced. The service life of the lubricating grease prepared by the method is obviously prolonged, and the grease replacement period is prolonged from 1.5-3 kilometres to 6 kilometres when the lubricating grease is applied to a commercial wheel hub bearing.
Drawings
FIG. 1 is a schematic diagram of the process steps for preparing a lithium mineral oil-based grease;
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Example 1: a lithium-based mineral oil grease comprising the following components:
base oil: 500Kg of mixed oil of MVI500 oil and MVI650 oil, wherein the MVI500 oil accounts for 55%, the MVI650 oil accounts for 45%, and the viscosity of the mixed oil at 100 ℃ is 11.28mm 2/s.
A thickening agent: the fatty acid lithium soap is obtained by saponifying a mixture of 12-hydroxystearic acid and stearic acid, lithium hydroxide and water, and 50Kg of 12-hydroxystearic acid, 10Kg of stearic acid, 9.0Kg of lithium hydroxide monohydrate and 10Kg of water are prepared.
Structure improving agent: 1.5Kg of a styrene-ethylene-propylene-styrene block copolymer.
Antioxidant: 2.0Kg of octyldiphenylamine.
Antirust agent: 1.1Kg of barium dinonyl naphthalene sulfonate.
The preparation process of the mineral oil lithium-based lubricating grease, as shown in figure 1, comprises the following steps:
s1: 250Kg of base oil, 50Kg of 12-hydroxystearic acid, 10Kg of stearic acid and 1.5Kg of styrene-ethylene-propylene-styrene block copolymer were put into a reaction vessel, stirred and heated.
S2: when the temperature rises to 60 ℃, 9.0Kg of lithium hydroxide monohydrate and 10Kg of water are added, and the kettle cover is closed and then heated for saponification reaction.
S3: heating to 150-160 deg.c and maintaining the temperature for reaction for 1 hr.
S4: and continuously heating to 170-180 ℃, and beginning to release pressure and discharge steam, wherein the highest refining temperature is 200-215 ℃.
S5: and (3) heating to 200-215 ℃, simultaneously pumping the high-temperature material and 100Kg of base oil for quenching in the reaction kettle into a quenching mixer, controlling the temperature of the quenched material to be 170-190 ℃, and feeding the material into a cooling kettle.
S6: and adding 150Kg of base oil after the materials in the cooling kettle are in a grease shape, performing circular shearing, and homogenizing to a blending kettle by a high-pressure homogenizer when the temperature is reduced to 110-130 ℃.
S7: cooling to 70-90 deg.c, adding 2.0Kg octyl diphenylamine and 1.1Kg barium dinonyl naphthalene sulfonate, regulating the consistency of the lubricating grease to be qualified, and degassing to obtain the lubricating grease product.
Example 2: a lithium-based mineral oil grease comprising the following components:
base oil: 510Kg MVI650 oil with a viscosity of 13.73mm at 100 ℃2/s。
A thickening agent: the lithium fatty acid soap was obtained by saponifying a mixture of 12-hydroxystearic acid and stearic acid, lithium hydroxide and water, to prepare 43Kg of 12-hydroxystearic acid, 11Kg of stearic acid, 8.3Kg of lithium hydroxide monohydrate and 9.2Kg of water.
Structure improving agent: 2.2Kg of a styrene-ethylene-propylene-styrene block copolymer.
Antioxidant: 2.0Kg of octyldiphenylamine.
Antirust agent: 1.1Kg of dodecenylsuccinic acid.
The preparation process of the mineral oil lithium-based lubricating grease, as shown in figure 1, comprises the following steps:
s1: 240Kg of base oil, 43Kg of 12-hydroxystearic acid, 11Kg of stearic acid and 2.2Kg of styrene-ethylene-propylene-styrene block copolymer were put into a reaction vessel, stirred and heated.
S2: when the temperature rises to 60 ℃, 8.3Kg of lithium hydroxide monohydrate and 9.2Kg of water are added, and the kettle cover is closed and then heated for saponification reaction.
S3: heating to 150-160 deg.c and maintaining the temperature for reaction for 1 hr.
S4: and continuously heating to 170-180 ℃, and beginning to release pressure and discharge steam, wherein the highest refining temperature is 200-215 ℃.
S5: and (3) heating to 200-215 ℃, simultaneously pumping the high-temperature material and 95Kg of base oil for quenching in the reaction kettle into a quenching mixer, controlling the temperature of the quenched material to be 170-190 ℃, and feeding the material into a cooling kettle.
S6: and adding 155Kg of base oil after the materials in the cooling kettle are in a grease shape, circularly shearing, and homogenizing to a mixing kettle by a high-pressure homogenizer when the temperature is reduced to 110-130 ℃.
S7: cooling to 70-90 deg.c, adding 2.0Kg octyl diphenylamine and 1.1Kg dodecenyl succinic acid, regulating the consistency of the lubricating grease to be qualified, and degassing to obtain the lubricating grease product.
Example 3: a lithium-based mineral oil grease comprising the following components:
base oil: 493Kg of MVI500 base oil having a viscosity of 2/s at 100 ℃ of 13.73 mm.
A thickening agent: the lithium fatty acid soap is obtained by saponifying a mixture of 12-hydroxystearic acid and stearic acid, lithium hydroxide and water, and 58Kg of 12-hydroxystearic acid, 12Kg of stearic acid, 10.3Kg of lithium hydroxide monohydrate and 12Kg of water are prepared.
Structure improving agent: 1.0Kg of a styrene-ethylene-propylene-styrene block copolymer.
Antioxidant: 2.0Kg of t-butyl-p-cresol.
Antirust agent: 1.1Kg of benzotriazole.
The preparation process of the mineral oil lithium-based lubricating grease, as shown in figure 1, comprises the following steps:
s1: 240Kg of base oil, 58Kg of 12-hydroxystearic acid, 12Kg of stearic acid and 1.0Kg of styrene-ethylene-propylene-styrene block copolymer were put into a reaction vessel, stirred and heated.
S2: when the temperature rises to 60 ℃, 10.3Kg of lithium hydroxide monohydrate and 12Kg of water are added, and the kettle cover is closed and then heated for saponification reaction.
S3: heating to 150-160 deg.c and maintaining the temperature for reaction for 1 hr.
S4: and continuously heating to 170-180 ℃, and beginning to release pressure and discharge steam, wherein the highest refining temperature is 200-215 ℃.
S5: and (3) heating to 200-215 ℃, simultaneously pumping the high-temperature material and 108Kg of base oil for quenching in the reaction kettle into a quenching mixer, controlling the temperature of the quenched material to be 170-190 ℃, and feeding the material into a cooling kettle.
S6: and adding 145Kg of base oil after the materials in the cooling kettle are in a grease shape, performing circular shearing, and homogenizing to a blending kettle by a high-pressure homogenizer when the temperature is reduced to 110-130 ℃.
S7: when the temperature is reduced to 70-90 ℃, 2.0Kg of tert-butyl-p-cresol and 1.1Kg of benzotriazole are added, the consistency of the lubricating grease is adjusted to be qualified, and the finished product of the lubricating grease is obtained after degassing.
Comparative example 1:
250Kg of base oil (viscosity at 100 ℃ is 11.28mm2/s), 50Kg of 12-hydroxystearic acid and 10Kg of stearic acid are put into a reaction kettle, stirred and heated to 60 ℃, and 9.0Kg of lithium hydroxide monohydrate and 10Kg of water are added. And sealing the kettle cover, heating to 150-160 ℃, and carrying out heat preservation reaction for 1 hour. And continuously heating to 170-180 ℃, releasing pressure and discharging water vapor, heating to 200-215 ℃, simultaneously pumping the high-temperature material and 100Kg of base oil for quenching in the reaction kettle into a quenching mixer, controlling the temperature of the quenched material to be 170-190 ℃, and feeding the material into a cooling kettle. And adding 150Kg of base oil after the materials in the cooling kettle are in a grease shape, performing circular shearing, and homogenizing to a blending kettle by a high-pressure homogenizer when the temperature is reduced to 110-130 ℃. Cooling to 70-90 deg.c, adding polyisobutylene 1.5Kg, octyl diphenylamine antioxidant 2.0Kg and barium dinonyl naphthalene sulfonate 1.1Kg, regulating the consistency of the lubricating grease to be qualified, and degassing to obtain the lubricating grease product.
Comparative example 2:
250Kg of base oil (viscosity at 100 ℃ is 11.28mm2/s), 50Kg of 12-hydroxystearic acid and 10Kg of stearic acid are put into a reaction kettle, stirred and heated to 60 ℃, and 9.0Kg of lithium hydroxide monohydrate and 10Kg of water are added. And sealing the kettle cover, heating to 150-160 ℃, and carrying out heat preservation reaction for 1 hour. And continuously heating to 170-180 ℃, releasing pressure and discharging water vapor, heating to 200-215 ℃, simultaneously pumping the high-temperature material and 100Kg of base oil for quenching in the reaction kettle into a quenching mixer, controlling the temperature of the quenched material to be 170-190 ℃, and feeding the material into a cooling kettle. Adding 140Kg of base oil after the materials in the cooling kettle are in a grease shape, circularly shearing, and homogenizing to a mixing kettle by a high-pressure homogenizer when the temperature is reduced to 110-130 ℃. When the temperature is reduced to 70-90 ℃, 1.5Kg of ethylene-propylene copolymer (pre-melted by 10Kg of base oil), 2.0Kg of octyl diphenylamine antioxidant and 1.1Kg of barium dinonyl naphthalene sulfonate antirust agent are added, the consistency of the lubricating grease is adjusted to be qualified, and the finished lubricating grease is obtained after degassing.
Comparative experiment: physical and chemical experiments were carried out on the greases of examples 1 to 3 and the greases of comparative examples 1 to 2, and the results obtained are shown in Table 1.
TABLE 1
The index adopts the change value of the penetration after cutting for one hundred thousand times of the lubricating grease to evaluate the anti-shearing performance, and adopts the weight loss rate of the water-resistant spray to evaluate the adhesion. As can be seen from sample inspection data of examples and comparative examples, compared with the lithium-based lubricating grease added with a common tackifier, the structurally-enhanced lithium-based lubricating grease prepared by the invention has the advantages that the shearing resistance and the adhesion performance are obviously improved, the leakage is reduced by about 50%, and the service life of the lubricating grease is effectively prolonged.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (9)
1. A lithium-based mineral oil grease comprising, in weight percent: 85-92% of base oil, 8-14% of thickening agent, 0.1-0.5% of structure improver, 0.3-0.5% of antioxidant and 0.1-0.3% of antirust agent.
2. The lithium-based mineral oil grease of claim 1, wherein: the base oil has a viscosity of 8.5-16 mm at 100 DEG C2One or more of paraffin-based mineral oil, intermediate-based mineral oil or naphthenic-based mineral oil in the second step.
3. The lithium-based mineral oil grease of claim 1, wherein: the thickening agent is fatty acid lithium soap which is a product obtained by saponification of fatty acid and lithium hydroxide, and the fatty acid is a mixture of 12-hydroxystearic acid and stearic acid.
4. The lithium-based mineral oil grease of claim 3, wherein: the stearic acid accounts for 10-30% of the weight of the fatty acid.
5. The lithium-based mineral oil grease of claim 1, wherein: the structure improver is a styrene-ethylene-propylene-styrene block copolymer, and the number average molecular weight of the block copolymer is 15-25 ten thousand.
6. The lithium-based mineral oil grease of claim 1, wherein: the antioxidant is amine or phenol antioxidant.
7. The lithium-based mineral oil grease of claim 1, wherein: the antirust agent is one of benzotriazole, barium dinonylnaphthalene sulfonate and dodecenylsuccinic acid.
8. A process for the preparation of a lithium mineral oil grease according to any one of claims 1 to 7, comprising the steps of:
s1: adding 30-50% of all base oil, fatty acid and a structure improver into a reaction kettle, fully mixing, heating and raising the temperature;
s2: after the temperature in the kettle rises to 60 ℃, adding lithium hydroxide monohydrate and water with the weight 1-2 times that of the lithium hydroxide monohydrate into the reaction kettle, and then starting to raise the temperature for saponification reaction;
s3: when the temperature is increased to 150 ℃ and 160 ℃, the reaction is carried out for 0.5 to 1 hour under the condition of heat preservation;
s4: continuously heating to 170-180 ℃, and releasing pressure to discharge water vapor in the reaction kettle;
s5: after refining, quickly cooling the high-temperature materials and 15-30% of base oil in the kettle through a quenching mixer, controlling the temperature to be 170-190 ℃ after quenching, and then transferring the quenched materials into a cooling kettle;
s6: continuously cooling the materials into grease, adding the residual base oil, performing circular shearing, and homogenizing by using a high-pressure homogenizer when the temperature is reduced to 110-130 ℃;
s7: and (3) cooling the material to 70-90 ℃, adding an antioxidant and an antirust agent, regulating and degassing to obtain a finished lubricating grease product.
9. The process according to claim 8, wherein the lithium-based lubricating grease comprises: in step S4, the maximum refining temperature of the reactor after pressure relief is controlled to be 200-215 ℃.
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| CN113549492A (en) * | 2021-06-18 | 2021-10-26 | 安美科技股份有限公司 | Lithium-based lubricating grease and saponification method thereof |
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