CN117070266A - High-base number composite calcium sulfonate-based lubricating grease composition and preparation method thereof - Google Patents

High-base number composite calcium sulfonate-based lubricating grease composition and preparation method thereof Download PDF

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Publication number
CN117070266A
CN117070266A CN202310769981.5A CN202310769981A CN117070266A CN 117070266 A CN117070266 A CN 117070266A CN 202310769981 A CN202310769981 A CN 202310769981A CN 117070266 A CN117070266 A CN 117070266A
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base
calcium sulfonate
grease
percent
base oil
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Inventor
刘文卓
艾合衣旦·巴衣斯
李小青
丁敏
郭小波
唐辉
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Xinjiang Jinxuechi Technology Co ltd
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Xinjiang Jinxuechi Technology Co ltd
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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
    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
    • C10M2201/0626—Oxides; Hydroxides; Carbonates or bicarbonates used as thickening agents
    • 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
    • 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
    • C10M2205/024—Propene
    • 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
    • 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
    • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/122—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms monocarboxylic
    • 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
    • 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
    • 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
    • C10M2219/046—Overbasedsulfonic acid salts
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/02—Pour-point; Viscosity index
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/08—Resistance to extreme temperature
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/10—Inhibition of oxidation, e.g. anti-oxidants
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Semi-solids; greasy

Abstract

The application discloses a high-base number composite calcium sulfonate-based lubricating grease composition and a preparation method thereof, and belongs to the technical field of lubricating grease preparation. The lubricating grease comprises the following components in percentage by mass: 4.8 to 7.3 percent of compound soap base, 1 to 2.7 percent of petroleum calcium sulfonate, 3 to 5 percent of high-base-number calcium sulfonate, 3 to 5 percent of acetic acid aqueous solution, 0.1 to 0.2 percent of antioxidant, 0.1 to 0.3 percent of antirust agent, 0.1 to 0.4 percent of adhesive and the balance of base oil; the preparation method comprises the following steps: firstly blending base oil, and carrying out phase inversion reaction on the blended base oil to generate non-Newtonian calcium sulfonate; then adding a composite soap base to prepare basic composite grease, adding a functional auxiliary agent into the basic composite grease, and finally carrying out homogenization post-treatment and degassing to obtain a lubricating grease product, wherein the lubricating grease product has better high-low temperature lubricity, extreme pressure abrasion resistance, mechanical stability, antioxidant rust resistance, long service life, safety and environmental protection. In addition, the modified polypropylene has good low-temperature fluidity, can be widely applied to low-temperature areas, and breaks through the obstruction of severe cold to agricultural production.

Description

High-base number composite calcium sulfonate-based lubricating grease composition and preparation method thereof
Technical Field
The application belongs to the technical field of grease preparation, and particularly relates to a high-base number composite calcium sulfonate-based grease composition and a preparation method thereof.
Background
In the fifties of the twentieth century, high drop point calcium sulfonate grease using calcium sulfonate as a thickener began to appear, but the oil-soluble newtonian calcium sulfonate solution used at this time has a small thickening ability and therefore has not been effectively popularized. In the last seventies of the century, a method for converting Newtonian calcium sulfonate solution into non-Newtonian calcium sulfonate with thixotropic property is invented, and a calcium sulfonate overbasing technology is added to prepare the overbased calcium sulfonate grease. The composite calcium sulfonate-based grease prepared by compositing the non-Newtonian high-base-number calcium sulfonate soap and other fatty acid salts is effectively improved in low-temperature pumping performance until the middle eighties, and meanwhile has certain high-low temperature performance, mechanical stability, oxidation stability, water resistance, corrosion resistance, rust resistance and extreme pressure wear resistance, and compared with the traditional grease, the comprehensive performance is greatly improved to a certain extent, so that the novel high-efficiency grease is called. However, the product is found to have the defects of poor low temperature resistance, weak colloid stability and the like in use, and is difficult to popularize and apply.
Through retrieval, the Chinese patent application number is: 201710531006.5, filing date: the application is named as 2017, 10 months and 13 days: a compound calcium sulfonate grease and its preparation method are provided. The composite calcium sulfonate base grease in the application comprises, by weight, 33.5-45.5% of a molecular alcohol phase inversion agent, 32.5-48.5% of a base oil and 11-15% of an organic acid phase inversion agent. According to the application, components and a preparation method are improved, so that the prepared product has good low-temperature flow property, the low-temperature property of the existing lubricating grease is improved, the comprehensive performance of the lubricating grease is still to be further improved, and meanwhile, the production process is complex.
For another example, chinese patent application number 201611103889.1, filing date: 26 days of 2017, 04 months, the application is named: a preparation method of composite calcium sulfonate grease. The base oils disclosed in this application include the following components: 21 to 50 parts by weight of high base number sulfonate, 0.3 to 5 parts by weight of calcium-containing inorganic matters and 0.01 to 8 parts by weight of sulfur-containing organic matters. Through improving the components and the proportion of the base oil, the prepared base oil has good viscosity-temperature characteristics, can meet the lubrication and sealing requirements of bearing equipment in the working environment with large day-night temperature difference, but still can not meet the various requirements of the equipment on the lubricating grease, and also limits the large-area use of the lubricating grease on other equipment to a certain extent.
Disclosure of Invention
1. Problems to be solved
The application aims to overcome the defects of single performance and poor comprehensive performance of the existing lubricating grease, and provides a high-base number composite calcium sulfonate-based lubricating grease composition and a preparation method thereof. By adopting the technical scheme of the application, the prepared lubricating grease can simultaneously meet the use requirements of extreme pressure wear resistance, corrosion resistance, rust resistance, high-speed pumping performance, low-temperature fluidity, environmental protection and safety of products, solves the problem of hardening of the lubricating grease when the lubricating grease is stored for a long time, improves the storage life, and has the advantages of simple preparation method, low cost and good economic benefit.
2. Technical proposal
In order to solve the problems, the technical scheme adopted by the application is as follows:
the application provides a high-base number composite calcium sulfonate-based lubricating grease composition, which comprises the following components in percentage by mass: 4.8 to 7.3 percent of compound soap base, 1 to 2.7 percent of petroleum calcium sulfonate, 3 to 5 percent of high-base-number calcium sulfonate, 3 to 5 percent of acetic acid aqueous solution, 0.1 to 0.2 percent of antioxidant, 0.1 to 0.3 percent of antirust agent, 0.1 to 0.4 percent of adhesive and the balance of base oil, wherein the mass ratio of water and acetic acid in the acetic acid aqueous solution is 2.2: (0.8-1.2).
Wherein the composite soap base comprises 0.5 to 1.58 percent of calcium dodecyl stearate, 4 to 5 percent of micro powder calcium carbonate and 0.3 to 0.72 percent of calcium hydroxide aqueous solution.
The base oil adopts 1570 ester base oil and intermediate base oil according to the proportion of 3.8: (0.8-1.2) and is prepared by blending. The intermediate base oil is selected from any one or two or more of N100, N150 and N250.
In the selection of the viscosity of the base oil, the base oil of the application has a kinematic viscosity of 96-100mm at 40 DEG C 2 And/s. The lubricating grease prepared from the high-viscosity base oil has good high-temperature stability, wide application range, poor colloid stability and oxidation stability, and high colloid stability and oxidation stability after thickening, but poor high-temperature stability. Furthermore, the applicant has carried out a great deal of tests on mineral oils of different types, such as synthetic hydrocarbon base oils, polyether base oils, etc., and having a certain viscosity span, according to the different types of base oils. In particular, the applicant has tested three 5 types of base oils (e.g., polyether base oils, synthetic hydrocarbon base oils, etc.) of the same viscosity, and analyzed these greases for similar viscosity and cone penetration at different temperatures. The results show that: the different types of base oil have larger influence on the consistence and similar viscosity of the lubricating grease, and the higher the viscosity index is used, the smaller the consistence and similar viscosity of the lubricating grease change along with the temperature, thereby being beneficial to the lubrication of equipment in a wide-temperature environment and ensuring stable operation. According to the application, mineral oil with different types and certain viscosity span is selected, calcium soap base grease is used as a starting point, the relation between base oil and rheological property is studied in depth by the system, and the essential cause of influence effect is studied in depth based on the level of ester molecules.
At the same soap content, the apparent viscosity of the grease changes in a temperature range of-20-70 ℃ and is related to the low temperature, and the important point for determining the low temperature performance of the grease is the pour point of the base oil, the viscosity and the viscosity index, the pour point is a key factor, and the viscosity effect is gradually highlighted only when the pour points are similar. As described above, the grease prepared from the high-viscosity base oil has better high-temperature stability, but has poorer colloid stability and oxidation stability, and simultaneously, as the viscosity of the base oil increases, the structural strength of the grease is firstly increased and then decreased, and the lower the structural strength, the better the thixotropic property of the component is, which is also closely related to the microstructure of the grease. The soap fiber structure formed by thickening the low-viscosity base oil is tightly wound and has smaller cavity volume, so that the soap fiber structure has higher colloid stability, and the soap fiber structure formed by the high-viscosity base oil is loose and has larger cavity volume, thereby being beneficial to continuously releasing the base oil and having good wear resistance and antifriction performance. In the aspect of oxidation stability, alkane belongs to saturated hydrocarbon and is relatively stable; whereas the carbon atoms to which the ring of the cycloalkane is attached to the side chain are susceptible to oxidation; the oxidation speed of aromatic hydrocarbon is slow, and after the benzene ring loses hydrogen atom, the aromatic hydrocarbon is easy to react with free radicals which initiate chain reaction to form stable aromatic hydrocarbon free radicals so as to terminate the chain reaction. Finally, the applicant selects 1570 ester lubricating oil and intermediate base oil according to 3.8: (0.8-1.2), and the balance between the viscosity and the high-temperature stability and the colloid stability of the base oil is found, the viscosity index of the base oil is higher, the pour point is low, and the temperature is less than-38 ℃ to-40 ℃.
As a further improvement of the application, the antioxidant is any one or two of 4, 4-methylene two and ZNDDC, and the applicant has found through extensive research that when the antioxidant is preferably the combination of 4, 4-methylene two and ZNDDC, and the mass ratio of 4, 4-methylene two and ZNDDC satisfies 1.2: (0.6-1), the grease and other components, especially complex soap base and micro powder calcium carbonate, have synergistic effect and perform optimal matching in the specific proportion, so that the high-low temperature performance, oxidation stability and mechanical stability of the obtained grease are obviously improved. In addition, the components of the lubricating grease are added with the adhesive and the rust inhibitor, so that the oxidation resistance and viscosity index performance of the lubricating grease product are improved, the service life of the lubricating grease is prolonged, the rate of deterioration and hardening in the use process is delayed, and the safety, stability and reliability in the use process are ensured.
As a further improvement of the application, the adhesive adopts a combination of polystyrene and ethylene-butylene, and the addition mass ratio of the polystyrene to the ethylene-butylene is 4.2: (1.4-2), the optimal mass ratio is 4.2:1.4. the applicant has carried out a great deal of experimental study in designing the proposal, and when the adhesive is added in the grease, and the adhesive is controlled in the proportion, the influence on the wear performance of the high-base number composite calcium sulfonate-based grease is better. In the test process, the applicant adopts an Shimadzu infrared spectrometer to track and analyze the components, chemical states and element contents of the lubricating grease. The result shows that the polystyrene and ethylene-butylene compound additive can obviously improve the wear resistance and the adhesive force of the high-base number composite calcium sulfonate-based lubricating grease. In the friction process, polystyrene can be adhered to the surface of the friction pair to form a physical protective film, and the physical protective film is cooperated and complemented with a chemical reaction film generated by ethylene-butylene, so that the polystyrene has excellent compounding synergy and adhesion performance.
As a further improvement of the grease, the application determines the specific types of the functional auxiliary agents by researching the types of the rest functional auxiliary agents, and the functional auxiliary agents can be well synergistic with components to play a role to the greatest extent and are not easy to generate side reactions when being added into the grease. Specifically, the antirust agent disclosed by the application adopts the dinonyl naphthalene calcium sulfonate, is a stable and excellent oil-soluble antirust agent, and the addition of the dinonyl naphthalene calcium sulfonate can wrap calcium carbonate particles tightly, so that the reaction between the dinonyl naphthalene calcium sulfonate and water and carbon dioxide in the air is isolated to a certain extent, and the dinonyl naphthalene calcium sulfonate can be neutralized with redundant acetic acid, so that the lubricating grease can be helped to thoroughly solve the hardening phenomenon. By optimizing the specific kinds of the above-mentioned auxiliary agents, the overall properties of the resulting grease product can be further improved.
On one hand, the high-base number composite calcium sulfonate-based lubricating grease disclosed by the application ensures the high-low temperature stability, colloid stability, oxidation stability and good wear resistance and antifriction performance of the lubricating grease by selecting the base oil with good compatibility, proper viscosity and lower pour point. On the other hand, the product of the application can also continue to work normally at a wide temperature, especially at extremely low temperatures. In addition, the selection of the additive considers the practical factors, and the application situation of the grease is most of extreme environments, so the requirements of wear resistance and lubricating property of the grease are researched, several adhesives capable of generating synergistic effect are found, the comprehensive property of the grease is greatly improved, the grease product with excellent comprehensive properties is prepared, the problem of single property of the existing grease is solved, and the application range of the grease is widened.
Secondly, the preparation method of the lubricating grease composition comprises the following steps:
step one, blending base oil;
step two, phase inversion is carried out by using the blended base oil to generate non-Newtonian calcium sulfonate;
step three, adding a composite soap base after phase inversion is completed to prepare basic composite grease;
step four, adding a functional auxiliary agent into the base grease, and homogenizing the obtained base grease;
and fifthly, degassing to obtain a lubricating grease product.
As a further improvement of the present application, the blending method of the base oil: the 1570 ester lubricating oil and the intermediate base oil are physically blended, and the kinematic viscosity of the blended base oil at 40 ℃ is controlled to be 96-100mm 2 S, pour point is-35 ℃ to-40 ℃.
The phase inversion method of the non-Newtonian calcium sulfonate comprises the following steps: adding part of base oil into a reaction kettle, adding part of base oil, petroleum calcium sulfonate and high-base-number calcium sulfonate into the reaction kettle, adding an aqueous solution of acetic acid at 100+/-5 ℃, and controlling the temperature to be 100+/-5 ℃ for reaction for 3 hours to obtain the inverted non-Newtonian sulfonic acid.
The petroleum calcium sulfonate can clean and disperse impurities in lubricating oil, has alkaline storage, good oil solubility and acid neutralization capability, can neutralize organic acid and inorganic acid in oil in time, and has excellent high-temperature detergency and thermal stability.
Furthermore, the reaction kettle is sealed at high pressure, and is provided with an observation port, so that the material liquid level condition in the reaction kettle can be monitored through the glass lens, and the reaction real-time condition can be mastered by an operator conveniently. Three layers of star-shaped stirring are arranged in the kettle, the reaction pressure is regulated to be 0.4-0.5MPa, and the high-order reaction does not overflow the kettle at the same time. The application adopts a one-step method for direct reaction, has low requirements on equipment, is simple and convenient to operate, reduces the production cost, has very stable product quality and has better application prospect.
As a further improvement of the application, in the step three, the high-temperature refining is carried out after the composite soap base is synthesized, the temperature of the composite soap base is controlled to be 180+/-5 ℃, then base oil is gradually added into the high-temperature composite soap base in 4 sections in a quenching mixer for full mixing, and finally, the base oil is regulated to form the base grease.
It should be noted that homogenization has a large influence on the microstructure and performance of the grease complex soap base. According to the application, the microstructure of the lubricating grease is ground by using the precise three-roller grinder at the distance of 25 mu m, the performance of the lubricating grease has obvious correlation with the microstructure of the composite soap base, and the change of the performance of the lubricating grease is caused by the increase of the specific surface area of the interaction of the composite soap base and the base oil due to grinding treatment, so that the cone penetration, dropping point, mechanical stability, colloid stability and rheological property of the lubricating grease are improved by the interaction force of the lubricating grease. The results show that: compared with the unground lubricating grease, the penetration degree is obviously reduced, the colloid stability and the structural strength are gradually increased along with the reduction of the grinding spacing, and the mechanical stability is reduced.
In the fourth step, firstly, adding an antirust agent into the obtained basic grease gradually until the temperature is reduced to below 90 ℃, then adding an antioxidant and an adhesive gradually after the mixture is sheared and mixed fully and uniformly, enabling the molecular structure recombination of each material to be more stable through a homogenizer, then carrying out degassing treatment, firstly, opening a vacuum pump to vacuumize the degassing tank, pumping the basic grease into the degassing tank by using a conveying pump under the condition that the vacuum reaches-0.8 MPa, stopping the vacuum pump when the material occupies 3/5 of the vacuum tank, returning to normal pressure, starting discharging, and repeating the operation for a plurality of times until the lubricating grease flows in a sheet shape or a thin flow shape. Finally, the lubricating grease product of the application is obtained.
The lubricating grease composition prepared by the application is particularly suitable for being used in a high-temperature environment, and the components, the proportion and the preparation process of the lubricating grease composition are optimally designed, so that the obtained lubricating grease product can keep good lubricity under severe working conditions and low-temperature weather conditions, the lubricating and sealing requirements of the high-base-number composite calcium sulfonate-based lubricating grease in a working environment with large day-night temperature difference are met, the service life of equipment is prolonged, and the lubricating grease composition has the advantages of good shearing reversibility, high-low temperature adaptability, extreme pressure wear resistance, rust resistance, good compatibility with other grease and the like. The lubricating grease disclosed by the application can be widely applied to Xinjiang areas, has good market feedback, has the characteristics of low temperature resistance, easiness in application, good adhesion, excellent water spray resistance and high cost performance, can protect equipment for a long time, and has a lubricating effect equivalent to that of similar products at home and abroad.
3. Advantageous effects
Compared with the prior art, the application has the beneficial effects that:
the lubricating grease composition prepared by the application is especially suitable for use in a high-temperature environment, and the prepared lubricating grease can simultaneously meet the use requirements of extreme pressure wear resistance, corrosion resistance, rust resistance, high-speed pumping performance, low-temperature fluidity, environmental protection and safety of products and the like by optimally designing the components, the proportion and the preparation process of the lubricating grease composition, and solves the problems of single performance and poor comprehensive performance of the conventional lubricating grease, so that the obtained lubricating grease product can keep better lubricity under severe working conditions and low-temperature climatic conditions, meet the lubricating and sealing requirements of high-base-number composite calcium sulfonate-based lubricating grease under working environments with large day-night temperature differences, and prolong the service life of equipment. In addition, the product of the application has the advantages of good shearing reversibility, high and low temperature adaptability, extreme pressure abrasion resistance, rust resistance, good compatibility with other grease and the like.
The preparation process of the lubricating grease provided by the application is simple and convenient to operate and low in cost, the prepared lubricating grease can be widely applied to Xinjiang areas, and has good market feedback, and the lubricating grease has the characteristics of low temperature resistance, easiness in smearing, good adhesiveness, excellent water spray resistance and high cost performance, can protect equipment for a long time, and has a lubricating effect equivalent to that of similar products at home and abroad.
Detailed Description
The application is further described below in connection with specific embodiments.
Example 1
The components and preparation process of the lubricating grease composition of the embodiment are as follows:
step S1, blending base oil, wherein 1570 ester base oil and N100 are adopted according to the mass ratio of 3.8:1.0 physical blending, and controlling the kinematic viscosity of the blended base oil at 40 ℃ to 96mm 2 S, pour point-35 ℃.
S2, carrying out phase inversion reaction on 86.35% of base oil, 3% of high-base-number calcium sulfonate, 3.5% of acetic acid aqueous solution and 1.2% of petroleum calcium sulfonate to obtain non-Newtonian calcium sulfonate, controlling the reaction temperature to be 100 ℃, adjusting the reaction pressure to be 0.4MPa, and the reaction time to be 3 hours, wherein in the conversion process, the stirring speed is controlled to be 100r/min, and the stirring speed in the later period of the conversion stage is controlled to be 145r/min.
And S3, adding 0.8% of calcium dodecahydroxystearate, 0.5% of calcium hydroxide aqueous solution and 4% of micro-powder calcium carbonate into the prepared non-Newtonian calcium sulfonate in a segmented manner, blending into base grease, specifically controlling the temperature of the composite soap base to be about 180 ℃, then adding base oil into the high-temperature composite soap base in a quenching mixer in a segmented manner by 4 segments step by step, fully mixing, and carrying out dehydration homogenization and post-treatment to adjust the consistency of the base grease to 273/10 mm.
Step S4, gradually adding 0.2% of antirust agent into the base grease at the temperature lower than 90 ℃, adding 0.15% of antioxidant (the mass ratio of the 4, 4-methylene II to the ZNDDC is 1.2:0.6), fully shearing and uniformly mixing, gradually adding 0.3% of adhesive (the mass ratio of the polystyrene to the ethylene-butylene is 4.2:1.6), treating by using a homogenizer, and degassing to obtain the lubricating grease.
The obtained grease was tested for its correlation properties, and the test results are shown in tables 1 and 2.
Example 2
The components and preparation process of the lubricating grease composition of the embodiment are as follows:
step S1, blending base oil, wherein 1570 ester base oil and N150 are adopted according to the mass ratio of 3.8:1.2 physical blending, and controlling the kinematic viscosity of the blended base oil at 40 ℃ to 98mm 2 S, pour point-40 ℃.
S2, carrying out phase inversion reaction on 84.45% of base oil, 3.5% of high-base-number calcium sulfonate, 4.3% of acetic acid aqueous solution and 1.5% of petroleum calcium sulfonate to obtain non-Newtonian calcium sulfonate, controlling the reaction temperature to 95 ℃, adjusting the reaction pressure to 0.45MPa, and the reaction time to 3 hours, wherein in the conversion process, the stirring speed is controlled to be 110r/min, and the stirring speed in the later stage of the conversion stage is controlled to be 140r/min.
S3, adding 1% of calcium dodecahydroxystearate, 0.3% of calcium hydroxide aqueous solution and 4.5% of micro-powder calcium carbonate into the prepared non-Newtonian calcium sulfonate in a segmented manner, blending to form base grease, specifically, controlling the temperature of the composite soap base to be about 185 ℃, then adding base oil into the high-temperature composite soap base in a quenching mixer in a segmented manner by 4 segments, fully mixing, and carrying out dehydration homogenization and post-treatment to adjust the consistency of the base grease to be 262/10 mm.
Step S4, gradually adding 0.15% of antirust agent into the base grease at the temperature lower than 90 ℃, adding 0.1% of antioxidant (the mass ratio of the 4, 4-methylene to the ZNDDC is 1.2:0.7), fully shearing and uniformly mixing, gradually adding 0.2% of adhesive (the mass ratio of the polystyrene to the ethylene-butylene is 4.2:1.4), treating by using a homogenizer, and degassing to obtain the lubricating grease.
The obtained grease was tested for its correlation properties, and the test results are shown in tables 1 and 2.
Example 3
The components and preparation process of the lubricating grease composition of the embodiment are as follows:
step S1, blending base oil, wherein 1570 ester base oil and N250 are adopted according to the mass ratio of 3.8:0.8, and the kinematic viscosity of the blended base oil is controlled to be 99mm at 40 DEG C 2 S, pour point-35 ℃.
And S2, carrying out phase inversion reaction on 85.03% of base oil, 4.3% of high-base-number calcium sulfonate, 3.85% of acetic acid aqueous solution and 1% of petroleum calcium sulfonate to obtain non-Newtonian calcium sulfonate, controlling the reaction temperature to be 100 ℃, adjusting the reaction pressure to be 0.4MPa, and the reaction time to be 3 hours, wherein in the conversion process, the stirring speed is controlled to be 105r/min, and the stirring speed in the later period of the conversion stage is controlled to be 140r/min.
And S3, adding 0.8% of calcium dodecahydroxystearate, 0.4% of calcium hydroxide aqueous solution and 4.2% of micro-powder calcium carbonate into the prepared non-Newtonian calcium sulfonate in a segmented manner, blending to form base grease, specifically, controlling the temperature of the composite soap base to be about 180 ℃, then adding base oil into the high-temperature composite soap base in a quenching mixer in a segmented manner by 4 segments step by step, fully mixing, and carrying out dehydration homogenization and post-treatment to adjust the consistency of the base grease to be 290/10 mm.
Step S4, gradually adding an antirust agent 0.1% into the base grease at the temperature below 90 ℃, adding an antioxidant 0.17% (the mass ratio of the 4, 4-methylene II to the ZNDDC is 1.2:0.8), fully shearing and uniformly mixing, gradually adding an adhesive 0.15% (the mass ratio of the polystyrene to the ethylene-butylene is 4.2:2), treating by using a homogenizer, and degassing to obtain the lubricating grease. The obtained grease was tested for its correlation properties, and the test results are shown in tables 1 and 2.
Example 4
The components and preparation process of the lubricating grease composition of the embodiment are as follows:
step S1, blending base oil, wherein 1570 ester base oil and N100+N150 are combined, and the mass ratio of the two base oils is 3.8:0.9, and the kinematic viscosity of the blended base oil at 40 ℃ is controlled to be 100mm 2 S, pour point-38 ℃.
S2, carrying out phase inversion reaction on 82.21% of base oil, 4.6% of high-base-number calcium sulfonate, 4.4% of acetic acid aqueous solution and 2% of petroleum calcium sulfonate to obtain non-Newtonian calcium sulfonate, controlling the reaction temperature to 105 ℃, adjusting the reaction pressure to 0.5MPa, and controlling the reaction time to 3 hours, wherein in the conversion process, the stirring speed is controlled to be 100r/min, and the stirring speed in the later period of the conversion stage is controlled to be 150r/min.
S3, adding 1.2% of calcium dodecahydroxystearate, 0.6% of calcium hydroxide aqueous solution and 4.3% of micro-powder calcium carbonate into the prepared non-Newtonian calcium sulfonate in a segmented manner, blending to form base grease, specifically, controlling the temperature of the composite soap base to be about 175 ℃, then adding base oil into the high-temperature composite soap base in a quenching mixer in a segmented manner in 4 segments gradually, fully mixing, and carrying out dehydration homogenization and post-treatment to adjust the consistency of the base grease to 295/10 mm.
Step S4, gradually adding 0.23% of antirust agent into the base grease at the temperature lower than 90 ℃, adding 0.18% of antioxidant (the mass ratio of the 4, 4-methylene II to the ZNDDC is 1.2:0.9), fully shearing and uniformly mixing, gradually adding 0.28% of adhesive (the mass ratio of the polystyrene to the ethylene-butylene is 4.2:1.8), treating by using a homogenizer, and degassing to obtain the lubricating grease. The obtained grease was tested for its correlation properties, and the test results are shown in tables 1 and 2.
Example 5
The components and preparation process of the lubricating grease composition of the embodiment are as follows:
step S1, blending base oil, wherein 1570 ester base oil and N250 are adopted according to the mass ratio of 3.8:1, physical blending, and controlling the kinematic viscosity of the blended base oil at 40 ℃ to 98mm 2 S, pour point-37 ℃.
S2, carrying out phase inversion reaction on 84.58% of base oil, 3.1% of high-base-number calcium sulfonate, 4% of acetic acid aqueous solution and 1.1% of petroleum calcium sulfonate to obtain non-Newtonian calcium sulfonate, controlling the reaction temperature to 100 ℃, adjusting the reaction pressure to 0.4MPa, and controlling the reaction time to 3h, wherein in the conversion process, the stirring speed is controlled to be 110r/min, and the stirring speed in the later stage of the conversion stage is controlled to be 150r/min.
S3, adding 1.5% of calcium dodecahydroxystearate, 0.45% of calcium hydroxide aqueous solution and 4.7% of micro-powder calcium carbonate into the prepared non-Newtonian calcium sulfonate in a segmented manner, blending to form base grease, specifically, controlling the temperature of the composite soap base to be about 180 ℃, then adding base oil into the high-temperature composite soap base in a quenching mixer in a segmented manner in 4 segments gradually, fully mixing, and carrying out dehydration homogenization and post-treatment to adjust the consistency of the base grease to be 260/10 mm.
Step S4, gradually adding 0.12% of antirust agent into the base grease at the temperature lower than 90 ℃, adding 0.13% of antioxidant (the mass ratio of the 4, 4-methylene to the ZNDDC is 1.2:1), fully shearing and uniformly mixing, gradually adding 0.32% of adhesive (the mass ratio of the polystyrene to the ethylene-butylene is 4.2:), treating by using a homogenizer, and degassing to obtain the lubricating grease. The obtained grease was tested for its correlation properties, and the test results are shown in tables 1 and 2.
Example 6
The components and preparation process of the lubricating grease composition of the embodiment are as follows:
step S1, blending base oil, wherein 1570 ester base oil and N150 are adopted according to the mass ratio of 3.8:0.8, and the kinematic viscosity of the blended base oil at 40 ℃ is controlled to be 96mm 2 S, pour point-38 ℃.
S2, carrying out phase inversion reaction on 84.8% of base oil, 4.2% of high-base-number calcium sulfonate, 4.3% of acetic acid aqueous solution and 2.7% of petroleum calcium sulfonate to obtain non-Newtonian calcium sulfonate, controlling the reaction temperature to 100 ℃, adjusting the reaction pressure to 0.5MPa, and the reaction time to 3 hours, wherein in the conversion process, the stirring speed is controlled to 110r/min, and the stirring speed in the later stage of the conversion stage is controlled to 150r/min.
S3, adding 1.58% of calcium dodecahydroxystearate, 0.72% of calcium hydroxide aqueous solution and 5% of micro-powder calcium carbonate into the prepared non-Newtonian calcium sulfonate in a segmented manner, blending into base grease, specifically controlling the temperature of the composite soap base to be about 180 ℃, then adding base oil into the high-temperature composite soap base in a quenching mixer in a segmented manner in 4 segments gradually, fully mixing, and homogenizing to adjust the consistency of the base grease to be 305/10 mm.
Step S4, gradually adding 0.3% of antirust agent into the base grease at the temperature lower than 90 ℃, adding 0.2% of antioxidant (the mass ratio of antioxidant 4, 4-methylene II to ZNDDC is 1.2:0.9), fully shearing and uniformly mixing, gradually adding 0.4% of adhesive (the mass ratio of polystyrene to ethylene-butylene is 4.2:1.6), treating by using a homogenizer, and degassing to obtain the lubricating grease. The obtained grease was tested for its correlation properties, and the test results are shown in tables 1 and 2.
Comparative example 1
The components and the preparation process of the lubricating grease composition of the comparative example are as follows:
carrying out phase inversion reaction on 85.43% of synthetic hydrocarbon base oil, 4% of high-base-number calcium sulfonate, 3.5% of acetic acid aqueous solution and 1.2% of petroleum calcium sulfonate to obtain non-Newtonian calcium sulfonate; in the reaction, the reaction pressure is controlled to be 0.4MPa, the reaction temperature is 100 ℃, and the reaction time is 3 hours. Adding 0.8% of calcium dodecahydroxystearate, 0.5% of calcium hydroxide aqueous solution and 4% of micro-powder calcium carbonate into the prepared non-Newtonian calcium sulfonate in a segmented manner, blending into base grease, adjusting the consistency of the base grease to 260/10 mm, gradually adding 0.12% of antirust agent and 0.13% of antioxidant into the base grease after the temperature is reduced to below 90 ℃, wherein the mass ratio of the antioxidant 4, 4-methylene and ZNDDC is 1.2:1, after fully shearing and uniformly mixing, gradually adding 0.32% of adhesive, treating by using a homogenizer, and degassing to obtain the lubricating grease.
The obtained grease was tested for its correlation properties and the test results are shown in table 3. 100 # base oil and blend base oils used in the present application, the base performance versus table 4.
Comparative example 2
The components and the preparation process of the lubricating grease composition of the comparative example are as follows:
carrying out phase inversion reaction on 85.75% of synthetic hydrocarbon base oil, 3.5% of high-base-number calcium sulfonate, 3% of acetic acid aqueous solution and 1.5% of petroleum calcium sulfonate to obtain non-Newtonian calcium sulfonate; in the reaction, the reaction pressure is controlled to be 0.5MPa, the reaction temperature is 105 ℃, and the reaction time is 3 hours. Adding 1% of calcium dodecahydroxystearate, 0.3% of calcium hydroxide aqueous solution and 4.5% of micro powder calcium carbonate into the prepared non-Newtonian calcium sulfonate in a partitioning way, blending into basic grease, and adjusting the consistency of the basic grease to 263/10 mm. Gradually adding 0.15% of antirust agent and 0.1% of antioxidant into the base grease after the temperature is reduced to below 90 ℃, wherein the antioxidant is only added with ZNDDC, and after the mixture is fully sheared and uniformly mixed, gradually adding 0.2% of adhesive agent, treating by using a homogenizer, and degassing to obtain the lubricating grease.
The obtained grease was tested for its correlation properties and the test results are shown in table 3.
Comparative example 3
The components and the preparation process of the lubricating grease composition of the comparative example are as follows:
carrying out phase inversion reaction on 85.53% of synthetic hydrocarbon base oil, 4.3% of high-base-number calcium sulfonate, 3.35% of acetic acid aqueous solution and 1% of petroleum calcium sulfonate to obtain non-Newtonian calcium sulfonate; in the reaction, the reaction pressure is controlled to be 0.4MPa, the reaction temperature is 100 ℃, and the reaction time is 3 hours. Adding 0.8% of calcium dodecahydroxystearate, 0.4% of calcium hydroxide aqueous solution and 4.2% of micro powder calcium carbonate into the prepared non-Newtonian calcium sulfonate in a partitioning way, blending to obtain base grease, and adjusting the consistency of the base grease to 305/10 mm. Gradually adding 0.1% of antirust agent and 0.17% of antioxidant into the base grease when the temperature is reduced to below 90 ℃, wherein the mass ratio of antioxidant 4, 4-methylene two to ZNDDC is 1.5:1, after fully shearing and uniformly mixing, gradually adding 0.15% of adhesive, treating by using a homogenizer, and degassing to obtain the lubricating grease.
The obtained grease was tested for its correlation properties and the test results are shown in table 3.
Comparative example 4
The components and the preparation process of the lubricating grease composition of the comparative example are as follows:
86.21% of synthesized hydrocarbon base oil, 2.6% of high-base-number calcium sulfonate, 2.4% of acetic acid aqueous solution and 2% of petroleum calcium sulfonate are subjected to phase inversion reaction to obtain non-Newtonian calcium sulfonate; the reaction pressure is controlled to be 0.5MPa, the reaction temperature is 100 ℃, and the reaction time is 3 hours. And (3) adding 1.2% of calcium dodecahydroxystearate, 0.6% of calcium hydroxide aqueous solution and 4.3% of micro-powder calcium carbonate into the prepared non-Newtonian calcium sulfonate in a partitioning way, blending into base grease, and adjusting the consistency of the base grease to 300/10 mm. And gradually adding 0.23% of antirust agent and 0.18% of antioxidant into the base grease after the temperature is reduced to below 90 ℃, wherein the antioxidant is only added with 4, 4-methylene II, and after the antioxidant is fully sheared and uniformly mixed, gradually adding 0.28% of adhesive, treating by adopting a homogenizer, and degassing to obtain the lubricating grease.
The obtained grease was tested for its correlation properties and the test results are shown in table 3.
Table 1 shows a comparison of the viscosities of the grease products obtained in the examples of the present application, similar to those of the prior art products. The existing product is specifically No. 2 high-base number composite calcium sulfonate grease.
Table 1 comparison of the viscosity of the grease products obtained in the examples with the prior art products
Table 2 results of detecting Performance indicators of greases obtained in examples
As can be seen from Table 1, the high-base-number composite calcium sulfonate grease obtained by the application has better stability and antioxidation characteristics, and is suitable for use in a sports machine with high movement precision, high bearing capacity requirement, high rotating speed and longer oil change period.
From the performance test indexes of examples 1 to 6 in table 2, it can be seen that the high-base number composite calcium sulfonate-based lubricating grease provided by the application has good low-temperature pumping performance, high-temperature resistance, extreme pressure wear resistance, oxidation resistance and rust resistance and mechanical stability. Is a lubricating product with excellent comprehensive performance. In addition, the preparation method of the high-base number composite calcium sulfonate grease is simple, can realize mass production, does not contain harmful substances, is safe and environment-friendly, and can meet a large amount of requirements on grease under extreme environments.
Table 3 shows the results of the performance index tests of the greases obtained in the comparative examples of the present application;
table 3 results of detection of greases obtained in comparative examples
Table 4 comparison of the properties of the synthetic ester base oils used in comparative example 1 with the base oils used in the present application
Project Synthetic ester oil The blend base oil of the application Test method
Viscosity/(mm) at 40 DEG C 2 /s) 180 96 GB/T 265
Pour point/. Degree.C 20 -38 GB/T 510
Flash point/. Degree.C 255 260 GB/T 3536
As can be seen from Table 3, the grease obtained by using the synthetic hydrocarbon as the base oil has poor high-temperature stability and does not improve the lubricity and wear resistance of the grease. As can be seen from Table 4, the blended base oil used in the application has the advantages of good basic physicochemical properties, proper viscosity, low pour point and high flash point, and the base oil has good low-temperature fluidity and strong stability, and can obviously improve various properties of the lubricating grease when being compounded with other components.
As can be seen from the detection indexes of comparative examples 2 to 4, when the kinds or proportions of additives in the grease are changed, the antiwear, rust-preventing, and antioxidant properties of the grease are lowered. The type and proportion of the additive are most suitable, and the prepared lubricating grease has more excellent performance.
In summary, the high-base number composite calcium sulfonate-based lubricating grease provided by the application has been described through a series of examples and comparative examples, and has excellent comprehensive performance in a certain range. The related experiment technicians can appropriately change and combine the components and the method according to the actual working conditions without departing from the content and the scope of the application, increase and decrease unnecessary technical characteristics, and meet the requirements of actual application.
More specifically, although exemplary embodiments of the present application have been described herein, the present application is not limited to these embodiments, but includes any and all embodiments that have been modified, omitted, e.g., combined, adapted, and/or substituted between the various embodiments, as would be recognized by those skilled in the art in light of the foregoing detailed description. The limitations in the claims are to be interpreted broadly based on the language employed in the claims and not limited to examples described in the foregoing detailed description or during the prosecution of the application, which examples are to be construed as non-exclusive. Any steps recited in any method or process claims may be executed in any order and are not limited to the order presented in the claims. The scope of the application should, therefore, be determined only by the appended claims and their legal equivalents, rather than by the descriptions and examples given above.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. In case of conflict, the present specification, definitions, will control. Where a rate, pressure, temperature, time, or other value or parameter is expressed as a range, preferred range, or as a range bounded by a list of upper and lower preferred values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, a range of 1-50 should be understood to include any number, combination of numbers, or subranges of numbers selected from 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, or 50, as well as all fractional values between the integers described above, such as 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, and 1.9. Regarding sub-ranges, specifically considered are "nested sub-ranges" that extend from any end point within the range. For example, the nested subranges of exemplary ranges 1-50 can include 1-10, 1-20, 1-30, and 1-40 in one direction, or 50-40, 50-30, 50-20, and 50-10 in another direction.

Claims (10)

1. The high-base number composite calcium sulfonate-based lubricating grease composition is characterized by comprising the following components in percentage by mass:
4.8 to 7.3 percent of compound soap base, 1 to 2.7 percent of petroleum calcium sulfonate, 3 to 5 percent of high-base-number calcium sulfonate, 3 to 5 percent of acetic acid aqueous solution, 0.1 to 0.2 percent of antioxidant, 0.1 to 0.3 percent of antirust agent, 0.1 to 0.4 percent of adhesive and the balance of base oil; wherein:
the composite soap base comprises 0.5-1.58% of calcium dodecyl stearate, 0.3-0.72% of calcium hydroxide aqueous solution and 4-5% of micro powder calcium carbonate;
the base oil adopts 1570 ester base oil and intermediate base oil according to the mass ratio of 3.8: (0.8-1.2) and is prepared by blending.
2. The high base number complex calcium sulfonate-based grease composition according to claim 1, wherein the mass ratio of water and acetic acid in the acetic acid aqueous solution satisfies 2.2: (0.8-1.2).
3. The high base number complex calcium sulfonate based grease composition according to claim 1, wherein the base oil has a kinematic viscosity of 96-100mm at 40 DEG C 2 S, pour point is-35 to-40 ℃, flash point is 260-300 ℃.
4. The high base number complex calcium sulfonate based grease composition of claim 1, wherein the intermediate base oil is selected from any one or a combination of two or more of N100, N150, N250.
5. A high base number complex calcium sulfonate based grease composition according to any one of claims 1-4, wherein the antioxidant is a combination of 4, 4-methylene two and ZNDDC; the antirust agent adopts calcium dinonyl naphthalene sulfonate, and the adhesive adopts a polymer composed of polystyrene and ethylene-butylene polymer.
6. The high base number complex calcium sulfonate based grease composition of claim 5, wherein the mass ratio of 4, 4-methylene two to ZNDDC satisfies 1.2: (0.6-1). The mass ratio of polystyrene to ethylene-butene polymer was 4.2: (1.4-2).
7. A method for preparing the high base number complex calcium sulfonate based grease composition according to any one of claims 1 to 6, comprising the steps of:
step one, blending base oil;
step two, carrying out phase inversion reaction on the blended base oil to generate non-Newtonian calcium sulfonate;
step three, adding a composite soap base after phase inversion is completed to prepare basic composite grease;
step four, adding a functional auxiliary agent into the composite grease, and carrying out homogenization post-treatment on the obtained basic grease;
and fifthly, degassing to obtain a lubricating grease product.
8. The method for preparing the high-base-number composite calcium sulfonate-based lubricating grease composition according to claim 7, wherein in the second step, base oil, high-base-number calcium sulfonate, petroleum calcium sulfonate and acetic acid aqueous solution are added into a reaction kettle, the reaction kettle is sealed under high pressure, three layers of star-shaped stirring is carried out in the reaction kettle, the reaction pressure is adjusted to be 0.4-0.5MPa, and the reaction kettle does not overflow during high-level reaction.
9. The method for preparing a high base number composite calcium sulfonate grease composition according to claim 7, wherein in the second step, the reaction temperature is controlled to be 100+/-5 ℃ for reaction, the phase-inverted high base number composite calcium sulfonate is obtained, in the conversion process, the stirring speed is controlled to be 100-110r/min, and in the later period of the conversion stage, the stirring speed is controlled to be 140-150r/min.
10. The method for preparing a high base number complex calcium sulfonate-based grease composition according to claim 9, wherein in the fourth step, an anti-rust agent, an antioxidant and an adhesive are sequentially added, wherein the anti-rust agent is gradually added to the obtained base grease after the temperature is reduced to below 90 ℃, and after the mixture is stirred uniformly, the anti-oxidant and the adhesive are gradually added, and the mixture is treated by a homogenizer.
CN202310769981.5A 2023-06-28 2023-06-28 High-base number composite calcium sulfonate-based lubricating grease composition and preparation method thereof Pending CN117070266A (en)

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