CN112111313A - Ultralow-temperature lubricating grease and preparation method thereof - Google Patents

Ultralow-temperature lubricating grease and preparation method thereof Download PDF

Info

Publication number
CN112111313A
CN112111313A CN202011040005.9A CN202011040005A CN112111313A CN 112111313 A CN112111313 A CN 112111313A CN 202011040005 A CN202011040005 A CN 202011040005A CN 112111313 A CN112111313 A CN 112111313A
Authority
CN
China
Prior art keywords
silicone oil
parts
lubricating grease
temperature
ultralow
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202011040005.9A
Other languages
Chinese (zh)
Other versions
CN112111313B (en
Inventor
高巍
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Harbin Sino Japanese Oil Chemical Industry Co ltd
Shanghai Hutou Chemical Co ltd
Original Assignee
Harbin Sino Japanese Oil Chemical Industry Co ltd
Shanghai Hutou Chemical Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Harbin Sino Japanese Oil Chemical Industry Co ltd, Shanghai Hutou Chemical Co ltd filed Critical Harbin Sino Japanese Oil Chemical Industry Co ltd
Priority to CN202011040005.9A priority Critical patent/CN112111313B/en
Publication of CN112111313A publication Critical patent/CN112111313A/en
Application granted granted Critical
Publication of CN112111313B publication Critical patent/CN112111313B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • C10M2201/10—Compounds containing silicon
    • C10M2201/102—Silicates
    • C10M2201/103—Clays; Mica; Zeolites
    • C10M2201/1036—Clays; Mica; Zeolites 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
    • C10M2205/028—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms
    • C10M2205/0285—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms used as base material
    • 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
    • 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
    • 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
    • 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
    • C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2213/06—Perfluoro polymers
    • C10M2213/062—Polytetrafluoroethylene [PTFE]
    • 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
    • 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
    • C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04—Siloxanes with specific structure
    • C10M2229/042—Siloxanes with specific structure containing aromatic substituents
    • C10M2229/0425—Siloxanes with specific structure containing aromatic substituents used as base material

Abstract

The invention discloses ultralow-temperature lubricating grease which comprises, by weight, 60-200 parts of base oil, 50-90 parts of silicone oil, 10-20 parts of a thickening agent, 5-20 parts of a saponification reaction agent, 1-8 parts of an additive and 1-5 parts of an auxiliary additive. The silicone oil is phenyl silicone oil, the base oil is a compound mixed oil of PAO4 and PAO8, and the thickening agent is a compound mixture of lithium soap and organic bentonite. According to the invention, through the restriction on the proportion of the base oil and the silicone oil, the restriction on the weight ratio of the thickening agent and the compounding manner of various additives, the prepared ultralow-temperature lubricating grease has excellent pour point, softness and low-temperature torque, can be effectively used for a long time, is suitable for being popularized and used as ultralow-temperature lubricating grease in the field of lubricating grease, and has wide development prospect.

Description

Ultralow-temperature lubricating grease and preparation method thereof
Technical Field
The invention relates to the field of lubricating grease, in particular to ultralow-temperature lubricating grease and a preparation method thereof.
Background
The lubricating grease is a thick grease-like semisolid, is a composite oil substance, is mostly used for a friction part of an apparatus, plays roles of lubricating, protecting and sealing, can also be used for a metal surface, and plays roles of filling a gap and preventing rust. The thickening agent keeps the oil at the position needing lubrication and protection, and releases the oil under the load pressure or at a certain temperature, thereby playing the roles of lubrication and protection. It is solid-like at normal temperature and at rest, can keep its own form and does not flow, can adhere to metal without sliding, and can flow like liquid at a certain temperature or under a certain high pressure. When flowing, it lubricates and reduces friction and wear on the moving surfaces, and when returning to ambient temperature or when the pressure ceases, it returns to a certain consistency.
The low-temperature lubricating grease is specially used in the environments of low temperature, high load pressure, high chemical corrosion and the like, generally has excellent temperature resistance, durability and a good use temperature range, is added with a structure improver, an antioxidant additive and a special antiwear additive, and is mainly used for equipment or machinery working in the environments of low temperature and high pressure.
In some working environments with lower temperature, such as aerospace, arctic probes and the like, more requirements are put on the low-temperature performance of the lubricating grease. In order to ensure the flight safety of aviation airplanes and the normal use of arctic scientific exploration equipment, the low-temperature lubricating grease not only needs to have strong low-temperature resistance, but also needs to have good oxidation resistance and wear resistance.
However, in the process of implementing the technical solution of the invention in the embodiments of the present application, the inventors of the present application find that the above-mentioned technology has at least the following technical problems:
the prior art (CN103525510B) relies on the low temperature stability of PAO, and combines PAO with mineral oil as base oil to prepare a grease product that can perform a lubricating effect at low temperature at low cost. But is limited by poor lubricating property and low-temperature resistance of mineral oil, and the prepared low-temperature lubricating grease has large low-temperature torque and small adaptive temperature range and cannot meet the requirement of lower temperature (-65 ℃).
Therefore, the present invention has been made to solve the above problems, and an investigation on an ultra-low temperature grease and a preparation method thereof has been made, which can provide stable lubricating performance at an ambient temperature of-65 ℃, is not easily frozen, and maintains good softness and wear resistance.
Disclosure of Invention
In order to solve the problems, the invention provides an ultralow-temperature lubricating grease in a first aspect, wherein the raw materials comprise the following components in parts by weight: 60-200 parts of base oil, 50-90 parts of silicone oil, 10-20 parts of a thickening agent, 5-20 parts of a saponification reaction agent, 1-8 parts of an additive and 1-5 parts of an auxiliary additive.
As a preferred embodiment, the base oil is one or a mixture of PAO4, PAO6, PAO8 and PAO10 in poly-alpha olefin; the silicone oil is at least one of phenyl silicone oil, amino silicone oil, dimethyl silicone oil, vinyl silicone oil and methyl silicone oil; the thickening agent is one or a mixture of lithium soap, organic bentonite, carbon black and silica gel fine powder; the saponification reactant is at least one of lithium hydroxide, potassium hydroxide, sodium hydroxide and calcium hydroxide; the additive is at least one of polytetrafluoroethylene, boron nitride, graphite, metal powder, hexadecanoic acid, tetradecanoic acid and boric acid; the auxiliary additive is at least one of di-tert-butyl-p-cresol, phenyl-alpha-aniline, dialkyl dithiophosphate, diphenylamine and hydroquinone.
As a preferred embodiment, the base oils are PAO4 and PAO8, the weight ratio of PAO4 to PAO8 is 2: 1.
as a preferable scheme, the silicone oil is phenyl silicone oil, and the weight ratio of the phenyl silicone oil to the base oil is (1-3): (2-4).
As a preferable mode, the phenyl silicone oil is phenyl silicone oil with average viscosity of 30 and phenyl silicone oil with average viscosity of 75.
In a preferred embodiment, the weight ratio of the phenyl silicone oil with the average viscosity of 30 to the phenyl silicone oil with the average viscosity of 75 is (2-4): (1-3).
As a preferable aspect, the ultralow temperature grease according to claim 6, wherein: the thickening agent is 12-lithium hydroxystearate, lithium stearate and organic bentonite, and the weight ratio of the 12-lithium hydroxystearate to the lithium stearate to the organic bentonite is (1-3): (1-3): (1-3).
As a preferable scheme, the additive is polytetrafluoroethylene with the average fineness of 20nm and polytetrafluoroethylene with the average fineness of 50nm, and the weight ratio of the polytetrafluoroethylene with the average fineness of 20nm to the polytetrafluoroethylene with the average fineness of 50nm is (1-3): (1-2).
As a preferred scheme, the auxiliary additive is di-tert-butyl-p-cresol and diphenylamine, and the weight ratio of the di-tert-butyl-p-cresol to the diphenol is 1: 1.
the second aspect of the invention provides a preparation method of ultralow temperature lubricating grease, which comprises the following steps: (1) weighing base oil, silicone oil, a thickening agent and an additive, heating to 50-120 ℃, stirring, and reacting for 1-3 hours; (2) adding a saponification reactant into the step (1), and then performing saponification reaction at the temperature of 100 ℃ and 130 ℃ for 4-8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 180-220 ℃ for high-temperature refining, wherein the reaction time is 2.5-5 hours, cooling to 100 ℃, finally adding an auxiliary additive, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease.
Has the advantages that: the invention provides ultralow-temperature lubricating grease and a preparation method thereof, and the prepared lubricating grease has excellent pour point, low-temperature torque, softness, low-temperature stability and chemical stability by limiting the viscosity and weight ratio of base oil and silicone oil, the proportion of a composite thickening agent and the fineness of an additive. The ultra-low temperature lubricating grease can be effectively used in a low temperature environment for a long time, is suitable for being popularized and used as ultra-low temperature lubricating grease in the field of lubricating grease, and has wide development prospect.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. 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 invention belongs. In case of conflict, the present specification, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable 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, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
In order to solve the problems, the invention provides an ultralow-temperature lubricating grease in a first aspect, wherein the raw materials comprise the following components in parts by weight: 60-200 parts of base oil, 50-90 parts of silicone oil, 10-20 parts of a thickening agent, 5-20 parts of a saponification reaction agent, 1-8 parts of an additive and 1-5 parts of an auxiliary additive.
The base oil, the thickening agent and the additive are main components of the lubricating grease, the base oil is a component with the largest content in the lubricating grease and also a component with a lubricating effect, and the performance of the base oil has a large influence on the performance of the lubricating grease. The thickener is an important component determining the performances of temperature resistance, stability, flexibility and the like of the lubricating grease, and takes base oil as a main medium to be dispersed in the whole lubricating grease. The thickening agent forms a framework of the whole lubricating grease, the base oil is fixed in the integral framework in a normal state, when the lubricating grease is subjected to high temperature and high pressure, the base oil is released from the framework to play a role in lubrication and protection, and the lubricating grease can recover a certain consistency when the lubricating grease returns to normal temperature and normal pressure. The additive is used as a supplement and plays a role in adding and supplementing in the synthesis of the lubricating grease, and the main function of the additive is to compensate the performance shortness board for the lubricating grease and perform functional addition.
In some preferred embodiments, the base oil is one or a mixture of PAO4, PAO6, PAO8, PAO10 in a poly-alpha olefin; the silicone oil is at least one of phenyl silicone oil, amino silicone oil, dimethyl silicone oil, vinyl silicone oil and methyl silicone oil; the thickening agent is one or a mixture of lithium soap, organic bentonite, carbon black and silica gel fine powder; the saponification reactant is at least one of lithium hydroxide, potassium hydroxide, sodium hydroxide and calcium hydroxide; the additive is at least one of polytetrafluoroethylene, boron nitride, graphite, metal powder, hexadecanoic acid, tetradecanoic acid and boric acid; the auxiliary additive is at least one of di-tert-butyl-p-cresol, phenyl-alpha-aniline, dialkyl dithiophosphate, diphenylamine and hydroquinone.
Poly-alpha olefin (PAO) is prepared by polymerizing ethylene to prepare alpha olefin, and further polymerizing and hydrogenating the alpha olefin, is excellent synthetic oil, has good viscosity property and low-temperature fluidity, has good high and low-temperature properties when used as a product, can resist emulsification, and has good thermal stability and chemical stability.
The saponification reaction is a necessary reaction in the preparation process of the lubricating grease, generally, the reaction is that oil ester substances and strong alkaline solution react to generate alcohol and glycerol, common alkali is sodium hydroxide, potassium hydroxide and the like, lithium hydroxide adopted in the application is used as an alkaline solvent participating in the saponification reaction and also used as a supplement of thickening agents such as lithium soap and the like, and the curing degree of the lubricating grease can be effectively improved under the synergistic effect of the alkaline solvent and the lithium hydroxide.
As a preferred embodiment, the base oils are PAO4 and PAO8, the weight ratio of PAO4 to PAO8 is 2: 1.
the PAOs in this application may be commercially available products such as the chevrons PAO4 and the chevrons PAO8 sold by shanghai qicheri international trade company.
In some preferred embodiments, the silicone oil is phenyl silicone oil, and the weight ratio of the phenyl silicone oil to the base oil is (1-3): (2-4). The phenyl silicone oil and the PAO are compounded, so that the low-temperature resistance, low-temperature fluidity, low-temperature stability, pressure resistance, lubricating property, stability, chemical stability and service life of the lubricating grease can be improved. The applicant speculates that the reason is that: a large number of phenyl groups contained in the phenyl silicone oil and a long straight chain alkane skeleton and a multi-side chain isoparaffin skeleton which are contained in the PAO have complementary synergistic effect, so that the performance of the lubricating grease is comprehensively improved. However, when the PAO content is too large, the high adhesion of the grease easily results in too high low temperature torque and hardness of the grease at low temperatures; when the amount of the phenyl silicone oil is too large, the service life of the lubricating grease is easily shortened, and the stability and chemical stability of the lubricating grease are reduced.
In some preferred embodiments, the phenyl silicone oil is a phenyl silicone oil having an average viscosity of 30 and a phenyl silicone oil having an average viscosity of 75.
In some preferred embodiments, the weight ratio of the phenyl silicone oil with the average viscosity of 30 to the phenyl silicone oil with the average viscosity of 75 is (2-4): (1-3). The phenyl silicone oil compounded with different viscosities can improve the compatibility of the lubricating grease with PAO oils of different models, reduce the flow resistance of the base oil at low temperature, and effectively improve the lubricity and softness of the lubricating grease at low temperature by adding the phenyl silicone oil. The applicant speculates that the reason is that: the synergistic effect of PAO4 and PAO8 in phenyl silicone oil and base oil can reduce the condensation resistance of the grease at low temperatures and reduce the rate of change of viscosity at low temperatures.
The phenyl silicone oil in the present application may be commercially available, for example, LX0401, LX0402 and LX0403 products produced by shanghai dragon xu chemical limited.
The unit of viscosity in this application is cSt, herein denominated centistokes, and is a kinematic viscosity unit, representing the ratio of the dynamic viscosity of a fluid to the density of the fluid at temperature, in international system of units (SI), the unit of kinematic viscosity is m2/s, 1cSt 10-6m2/s 1mm2/s, and can be determined according to the method described in GB/T256-88 or ASTM D445-96.
In some preferred embodiments, the thickener is 12-lithium hydroxystearate, lithium stearate and organic bentonite, and the weight ratio of the lithium stearate to the organic bentonite is (1-3): (1-3): (1-3).
The curing degree, stability, lubricity and low-temperature fluidity of the low-temperature lubricating grease can be considered at the same time by using the compound thickening agent of the 12-hydroxy lithium stearate, the lithium stearate and the organic bentonite. Only 12-lithium hydroxystearate is used as a thickening agent, so that the lubricating grease has high curing degree, high softness and poor stability; only lithium stearate is used as a thickening agent, and the produced lubricating grease has high lubricating property, poor fluidity and lower solidification degree. The organobentonite has better low-temperature rheological property, does not participate in phase transformation in the curing process, has small influence on the curing degree of the lubricating grease by temperature, and can effectively reduce the hardness of the lubricating grease at high and low temperatures. Moreover, because the bentonite is subjected to organic modification and has oleophylic hydrophobicity, the affinity of the whole compound thickening agent in the base oil is improved, so that the thickening agent can be quickly filled, an additional oleophylic suspension forming agent is not needed, and the influence of the forming agent on other properties of the lubricating grease is avoided.
The lithium 12-hydroxystearate and lithium stearate herein may be commercially available, for example, as the lithium 12-hydroxystearate and lithium stearate products in the environmental protection plastics additives series manufactured by lake Water chestnut lake News chemical Co.
The organobentonite in the present application may be commercially available, for example, the organobentonite product produced by Shijiazhu, Leishan mineral processing Co.
In some preferred embodiments, the additive is polytetrafluoroethylene with an average fineness of 20nm and polytetrafluoroethylene with an average fineness of 50nm, and the weight ratio of the polytetrafluoroethylene with the average fineness of 20nm to the polytetrafluoroethylene with the average fineness of 50nm is (1-3): (1-2).
Polytetrafluoroethylene (CAS number: 9002-84-0) powder compounded with different fineness can be quickly and effectively filled into all parts of base oil, no additional lipophilic suspension forming agent is needed, and the influence of the forming agent on the overall performance of the lubricating grease is avoided. The addition of the polytetrafluoroethylene can effectively improve the abrasion resistance and chemical stability of the lubricating grease. The polytetrafluoroethylene has extremely low mutual attraction among the polytetrafluoroethylene macromolecules and extremely low attraction of the surfaces of the polytetrafluoroethylene macromolecules to other molecules, and the absence of branched chains and cross chains provides a smooth molecular profile for the polytetrafluoroethylene. And the extremely short bond length of the C-F bond in the polytetrafluoroethylene ensures that the polytetrafluoroethylene molecular structure is stable and bond breakage is not easy to cause.
In some preferred embodiments, the auxiliary additive is di-tert-butyl-p-cresol and diphenylamine, and the weight ratio of di-tert-butyl-p-cresol and diphenol is 1: 1.
the complex of the di-tert-butyl-p-cresol (CAS number: 128-37-0) and the diphenylamine (CAS number: 122-39-4) has more remarkable effect on reducing the phenomenon of atom electron loss in the lubricating grease than the single use. Phenols and amines used as free radical scavengers can capture active free electrons, enable the active free electrons to become inactive electrons, and inhibit continuous electron losing reaction, and phenols contribute to the regeneration of amines and can inhibit atom electron losing reaction for a long time, and the synergistic effect of the phenols and the amines inhibits the electron losing activity of compound thickeners, such as bentonite and lithium stearate, so that the low-temperature stability of the low-temperature lubricating grease is improved.
The second aspect of the present invention provides a preparation method of the ultralow temperature grease, comprising the following steps: (1) weighing base oil, silicone oil, a thickening agent and an additive, heating to 50-120 ℃, stirring, and reacting for 1-3 hours; (2) adding a saponification reactant into the step (1), and then performing saponification reaction at the temperature of 100 ℃ and 130 ℃ for 4-8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 180-220 ℃ for high-temperature refining, wherein the reaction time is 2.5-5 hours, cooling to 100 ℃, finally adding an auxiliary additive, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease.
Examples
The technical solution of the present invention is described in detail by the following examples, but the scope of the present invention is not limited to all of the examples. The starting materials of the present invention are all commercially available unless otherwise specified.
Example 1
Embodiment 1 provides ultralow-temperature lubricating grease, which comprises the following raw materials, by weight, 60 parts of phenyl silicone oil (the phenyl silicone oil with the average viscosity of 30 and the phenyl silicone oil with the average viscosity of 75 are compounded in a weight ratio of 3: 2), 90 parts of PAO base oil (the PAO4 and the PAO8 are compounded in a weight ratio of 2: 1), 20 parts of a compound thickening agent (lithium 12-hydroxystearate, lithium stearate and organic bentonite are compounded in a weight ratio of 1: 1: 2), 20 parts of lithium hydroxide, 8 parts of polytetrafluoroethylene powder (polytetrafluoroethylene with the average fineness of 20nm and polytetrafluoroethylene with the average fineness of 50nm are compounded in a weight ratio of 3: 2), 2.5 parts of diphenylamine and 2.5 parts of di-tert-butyl-p-cresol.
The PAOs in this example are the products of chevrons PAO4 and chevrons PAO8 sold by shanghai qichering international trade company.
The phenyl silicone oil in this example is LX0401 and LX0402 products produced by shanghai dragon xu chemical limited.
The lithium 12-hydroxystearate and lithium stearate in this example are products of lithium 12-hydroxystearate and lithium stearate in the series of environmentally friendly plastic aids produced by the chemical company NwIthan, Tra lake, Huzhou.
The organic bentonite in this example is an organic bentonite product produced by Shijiazhuang, Cilishang, and Heshang mineral product processing Co.
The embodiment also provides a preparation method of the ultralow-temperature lubricating grease, which comprises the following steps: (1) weighing phenyl silicone oil, base oil, a thickening agent and polytetrafluoroethylene powder, heating to 100 ℃, stirring, and reacting for 3 hours; (2) adding lithium hydroxide into the step (1), and then performing saponification reaction at 120 ℃ for 8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 220 ℃ for high-temperature refining, wherein the reaction time is 3 hours, cooling to 100 ℃, finally adding di-tert-butyl-p-cresol and diphenylamine, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease. This grease was designated as R1.
Example 2
Embodiment 2 provides ultralow-temperature lubricating grease, which comprises the following raw materials, by weight, 50 parts of phenyl silicone oil (the phenyl silicone oil with the average viscosity of 30 and the phenyl silicone oil with the average viscosity of 75 are compounded in a weight ratio of 3: 2), 200 parts of PAO base oil (the PAO4 and the PAO8 are compounded in a weight ratio of 2: 1), 20 parts of a compound thickening agent (lithium 12-hydroxystearate, lithium stearate and organic bentonite are compounded in a weight ratio of 1: 1: 2), 20 parts of lithium hydroxide, 8 parts of polytetrafluoroethylene powder (polytetrafluoroethylene with the average fineness of 20nm and polytetrafluoroethylene with the average fineness of 50nm are compounded in a weight ratio of 3: 2), 2.5 parts of diphenylamine and 2.5 parts of di-tert-butyl-p-cresol.
The PAO used in this example was the same as in example 1.
The phenyl silicone oil used in this example was the same as in example 1.
The lithium 12-hydroxystearate and lithium stearate used in this example were the same as in example 1.
The organobentonite used in this example was the same as in example 1.
The embodiment also provides a preparation method of the ultralow-temperature lubricating grease, which comprises the following steps: (1) weighing phenyl silicone oil, base oil, a thickening agent and polytetrafluoroethylene powder, heating to 100 ℃, stirring, and reacting for 3 hours; (2) adding lithium hydroxide into the step (1), and then performing saponification reaction at 120 ℃ for 8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 220 ℃ for high-temperature refining, wherein the reaction time is 3 hours, cooling to 100 ℃, finally adding di-tert-butyl-p-cresol and diphenylamine, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease. This grease was designated as R2.
Example 3
Embodiment 3 provides ultralow-temperature lubricating grease, which comprises the following raw materials, by weight, 90 parts of phenyl silicone oil (the phenyl silicone oil with the average viscosity of 30 and the phenyl silicone oil with the average viscosity of 75 are compounded in a weight ratio of 3: 2), 60 parts of PAO base oil (the PAO4 and the PAO8 are compounded in a weight ratio of 2: 1), 20 parts of a compound thickening agent (lithium 12-hydroxystearate, lithium stearate and organic bentonite are compounded in a weight ratio of 1: 1: 2), 20 parts of lithium hydroxide, 8 parts of polytetrafluoroethylene powder (polytetrafluoroethylene with the average fineness of 20nm and polytetrafluoroethylene with the average fineness of 50nm are compounded in a weight ratio of 3: 2), 2.5 parts of diphenylamine and 2.5 parts of di-tert-butyl-p-cresol.
The PAO used in this example was the same as in example 1.
The phenyl silicone oil used in this example was the same as in example 1.
The lithium 12-hydroxystearate and lithium stearate used in this example were the same as in example 1.
The organobentonite used in this example was the same as in example 1.
The embodiment also provides a preparation method of the ultralow-temperature lubricating grease, which comprises the following steps: (1) weighing phenyl silicone oil, base oil, a thickening agent and polytetrafluoroethylene powder, heating to 100 ℃, stirring, and reacting for 3 hours; (2) adding lithium hydroxide into the step (1), and then performing saponification reaction at 120 ℃ for 8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 220 ℃ for high-temperature refining, wherein the reaction time is 3 hours, cooling to 100 ℃, finally adding di-tert-butyl-p-cresol and diphenylamine, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease. This grease was designated as R3.
Example 4
Embodiment 4 provides an ultralow-temperature lubricating grease, which comprises, by weight, 60 parts of phenyl silicone oil (the phenyl silicone oil having an average viscosity of 30 and the phenyl silicone oil having an average viscosity of 75 are compounded in a weight ratio of 4: 1), 90 parts of PAO base oil (the PAO4 and the PAO8 are compounded in a weight ratio of 2: 1), 20 parts of a compound thickener (lithium 12-hydroxystearate, lithium stearate and organobentonite are compounded in a weight ratio of 1: 1: 2), 20 parts of lithium hydroxide, 8 parts of polytetrafluoroethylene powder (polytetrafluoroethylene having an average fineness of 20nm and polytetrafluoroethylene having an average fineness of 50nm are compounded in a weight ratio of 3: 2), 2.5 parts of diphenylamine, and 2.5 parts of di-tert-butyl-p-cresol.
The PAO used in this example was the same as in example 1.
The phenyl silicone oil used in this example was the same as in example 1.
The lithium 12-hydroxystearate and lithium stearate used in this example were the same as in example 1.
The organobentonite used in this example was the same as in example 1.
The embodiment also provides a preparation method of the ultralow-temperature lubricating grease, which comprises the following steps: (1) weighing phenyl silicone oil, base oil, a thickening agent and polytetrafluoroethylene powder, heating to 100 ℃, stirring, and reacting for 3 hours; (2) adding lithium hydroxide into the step (1), and then performing saponification reaction at 120 ℃ for 8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 220 ℃ for high-temperature refining, wherein the reaction time is 3 hours, cooling to 100 ℃, finally adding di-tert-butyl-p-cresol and diphenylamine, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease. This grease was designated as R4.
Example 5
Embodiment 5 provides ultralow-temperature lubricating grease, which comprises the following raw materials, by weight, 60 parts of phenyl silicone oil (the phenyl silicone oil with the average viscosity of 30 and the phenyl silicone oil with the average viscosity of 75 are compounded in a weight ratio of 2: 3), 90 parts of PAO base oil (the PAO4 and the PAO8 are compounded in a weight ratio of 2: 1), 20 parts of a compound thickening agent (lithium 12-hydroxystearate, lithium stearate and organic bentonite are compounded in a weight ratio of 1: 1: 2), 20 parts of lithium hydroxide, 8 parts of polytetrafluoroethylene powder (polytetrafluoroethylene with the average fineness of 20nm and polytetrafluoroethylene with the average fineness of 50nm are compounded in a weight ratio of 3: 2), 2.5 parts of diphenylamine and 2.5 parts of di-tert-butyl-p-cresol.
The PAO used in this example was the same as in example 1.
The phenyl silicone oil used in this example was the same as in example 1.
The lithium 12-hydroxystearate and lithium stearate used in this example were the same as in example 1.
The organobentonite used in this example was the same as in example 1.
The embodiment also provides a preparation method of the ultralow-temperature lubricating grease, which comprises the following steps: (1) weighing phenyl silicone oil, base oil, a thickening agent and polytetrafluoroethylene powder, heating to 100 ℃, stirring, and reacting for 3 hours; (2) adding lithium hydroxide into the step (1), and then performing saponification reaction at 120 ℃ for 8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 220 ℃ for high-temperature refining, wherein the reaction time is 3 hours, cooling to 100 ℃, finally adding di-tert-butyl-p-cresol and diphenylamine, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease. This grease was designated as R5.
Example 6
Embodiment 6 provides ultralow-temperature lubricating grease, which comprises the following raw materials, by weight, 60 parts of phenyl silicone oil (the phenyl silicone oil with the average viscosity of 30 and the phenyl silicone oil with the average viscosity of 75 are compounded in a weight ratio of 3: 2), 90 parts of PAO base oil (the PAO4 and the PAO8 are compounded in a weight ratio of 2: 1), 20 parts of a compound thickening agent (lithium 12-hydroxystearate, lithium stearate and organic bentonite are compounded in a weight ratio of 3: 3: 1), 20 parts of lithium hydroxide, 8 parts of polytetrafluoroethylene powder (polytetrafluoroethylene with the average fineness of 20nm and polytetrafluoroethylene with the average fineness of 50nm are compounded in a weight ratio of 3: 2), 2.5 parts of diphenylamine and 2.5 parts of di-tert-butyl-p-cresol.
The PAO used in this example was the same as in example 1.
The phenyl silicone oil used in this example was the same as in example 1.
The lithium 12-hydroxystearate and lithium stearate used in this example were the same as in example 1.
The organobentonite used in this example was the same as in example 1.
The embodiment also provides a preparation method of the ultralow-temperature lubricating grease, which comprises the following steps: (1) weighing phenyl silicone oil, base oil, a thickening agent and polytetrafluoroethylene powder, heating to 100 ℃, stirring, and reacting for 3 hours; (2) adding lithium hydroxide into the step (1), and then performing saponification reaction at 120 ℃ for 8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 220 ℃ for high-temperature refining, wherein the reaction time is 3 hours, cooling to 100 ℃, finally adding di-tert-butyl-p-cresol and diphenylamine, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease. This grease was designated as R6.
Example 7
Embodiment 7 provides ultralow-temperature lubricating grease, which comprises the following raw materials, by weight, 60 parts of phenyl silicone oil (the phenyl silicone oil with the average viscosity of 30 and the phenyl silicone oil with the average viscosity of 75 are compounded in a weight ratio of 3: 2), 90 parts of PAO base oil (the PAO4 and the PAO8 are compounded in a weight ratio of 2: 1), 20 parts of a compound thickening agent (lithium 12-hydroxystearate, lithium stearate and organic bentonite are compounded in a weight ratio of 1: 1: 3), 20 parts of lithium hydroxide, 8 parts of polytetrafluoroethylene powder (polytetrafluoroethylene with the average fineness of 20nm and polytetrafluoroethylene with the average fineness of 50nm are compounded in a weight ratio of 3: 2), 2.5 parts of diphenylamine and 2.5 parts of di-tert-butyl-p-cresol.
The PAO used in this example was the same as in example 1.
The phenyl silicone oil used in this example was the same as in example 1.
The lithium 12-hydroxystearate and lithium stearate used in this example were the same as in example 1.
The organobentonite used in this example was the same as in example 1.
The embodiment also provides a preparation method of the ultralow-temperature lubricating grease, which comprises the following steps: (1) weighing phenyl silicone oil, base oil, a thickening agent and polytetrafluoroethylene powder, heating to 100 ℃, stirring, and reacting for 3 hours; (2) adding lithium hydroxide into the step (1), and then performing saponification reaction at 120 ℃ for 8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 220 ℃ for high-temperature refining, wherein the reaction time is 3 hours, cooling to 100 ℃, finally adding di-tert-butyl-p-cresol and diphenylamine, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease. This grease was designated as R7.
Example 8
Embodiment 8 provides ultralow-temperature lubricating grease, which comprises the following raw materials, by weight, 60 parts of phenyl silicone oil (the phenyl silicone oil with the average viscosity of 30 and the phenyl silicone oil with the average viscosity of 75 are compounded in a weight ratio of 3: 2), 90 parts of PAO base oil (the PAO4 and the PAO8 are compounded in a weight ratio of 2: 1), 20 parts of a compound thickening agent (lithium 12-hydroxystearate, lithium stearate and organic bentonite are compounded in a weight ratio of 1: 1: 2), 20 parts of lithium hydroxide, 8 parts of polytetrafluoroethylene powder (polytetrafluoroethylene with the average fineness of 20nm and polytetrafluoroethylene with the average fineness of 50nm are compounded in a weight ratio of 1: 1), 2.5 parts of diphenylamine and 2.5 parts of di-tert-butyl-p-cresol.
The PAO used in this example was the same as in example 1.
The phenyl silicone oil used in this example was the same as in example 1.
The lithium 12-hydroxystearate and lithium stearate used in this example were the same as in example 1.
The organobentonite used in this example was the same as in example 1.
The embodiment also provides a preparation method of the ultralow-temperature lubricating grease, which comprises the following steps: (1) weighing phenyl silicone oil, base oil, a thickening agent and polytetrafluoroethylene powder, heating to 100 ℃, stirring, and reacting for 3 hours; (2) adding lithium hydroxide into the step (1), and then performing saponification reaction at 120 ℃ for 8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 220 ℃ for high-temperature refining, wherein the reaction time is 3 hours, cooling to 100 ℃, finally adding di-tert-butyl-p-cresol and diphenylamine, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease. This grease was designated as R8.
Comparative example 1
Comparative example 1 provides an ultralow temperature lubricating grease, and the raw materials comprise, by weight, 150 parts of phenyl silicone oil (the phenyl silicone oil with the average viscosity of 30 and the phenyl silicone oil with the average viscosity of 75 are compounded in a weight ratio of 3: 2), 90 parts of PAO base oil (the PAO4 and the PAO8 are compounded in a weight ratio of 2: 1), 20 parts of a compound thickener (12-lithium hydroxystearate, lithium stearate and organic bentonite are compounded in a weight ratio of 1: 1: 2), 20 parts of lithium hydroxide, 8 parts of polytetrafluoroethylene powder (polytetrafluoroethylene with the average fineness of 20nm and compounded polytetrafluoroethylene with the average fineness of 50nm are compounded in a weight ratio of 3: 2), 2.5 parts of diphenylamine and 2.5 parts of di-tert-butyl-p-cresol.
The PAO used in this comparative example was the same as in example 1.
The phenyl silicone oil used in this comparative example was the same as in example 1.
The lithium 12-hydroxystearate and lithium stearate used in this comparative example were the same as in example 1.
The organobentonite used in this comparative example was the same as in example 1.
The comparative example also provides a preparation method of the ultralow temperature lubricating grease, which comprises the following steps: (1) weighing phenyl silicone oil, base oil, a thickening agent and polytetrafluoroethylene powder, heating to 100 ℃, stirring, and reacting for 3 hours; (2) adding lithium hydroxide into the step (1), and then performing saponification reaction at 120 ℃ for 8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 220 ℃ for high-temperature refining, wherein the reaction time is 3 hours, cooling to 100 ℃, finally adding di-tert-butyl-p-cresol and diphenylamine, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease. This grease was designated as D1.
Comparative example 2
Comparative example 2 provides ultralow-temperature lubricating grease, and the raw materials comprise, by weight, 60 parts of phenyl silicone oil (the phenyl silicone oil with the average viscosity of 30 and the phenyl silicone oil with the average viscosity of 75 are compounded in a weight ratio of 3: 2), 90 parts of PAO base oil (the PAO4 and the PAO8 are compounded in a weight ratio of 1: 2), 20 parts of a compound thickening agent (lithium 12-hydroxystearate, lithium stearate and organic bentonite are compounded in a weight ratio of 1: 1: 2), 20 parts of lithium hydroxide, 8 parts of polytetrafluoroethylene powder (polytetrafluoroethylene with the average fineness of 20nm and polytetrafluoroethylene with the average fineness of 50nm are compounded in a weight ratio of 3: 2), 2.5 parts of diphenylamine and 2.5 parts of di-tert-butyl-p-cresol.
The PAO used in this comparative example was the same as in example 1.
The phenyl silicone oil used in this comparative example was the same as in example 1.
The lithium 12-hydroxystearate and lithium stearate used in this comparative example were the same as in example 1.
The organobentonite used in this comparative example was the same as in example 1.
The comparative example also provides a preparation method of the ultralow temperature lubricating grease, which comprises the following steps: (1) weighing phenyl silicone oil, base oil, a thickening agent and polytetrafluoroethylene powder, heating to 100 ℃, stirring, and reacting for 3 hours; (2) adding lithium hydroxide into the step (1), and then performing saponification reaction at 120 ℃ for 8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 220 ℃ for high-temperature refining, wherein the reaction time is 3 hours, cooling to 100 ℃, finally adding di-tert-butyl-p-cresol and diphenylamine, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease. This grease was designated as D2.
Comparative example 3
Comparative example 3 provides ultralow-temperature lubricating grease, and the raw materials comprise, by weight, 60 parts of phenyl silicone oil (the phenyl silicone oil with the average viscosity of 30 and the phenyl silicone oil with the average viscosity of 75 are compounded in a weight ratio of 6: 1), 90 parts of PAO base oil (the PAO4 and the PAO8 are compounded in a weight ratio of 2: 1), 20 parts of a compound thickening agent (12-lithium hydroxystearate, lithium stearate and organic bentonite are compounded in a weight ratio of 1: 1: 2), 20 parts of lithium hydroxide, 8 parts of polytetrafluoroethylene powder (polytetrafluoroethylene with the average fineness of 20nm and compounded polytetrafluoroethylene with the average fineness of 50nm are compounded in a weight ratio of 3: 2), 2.5 parts of diphenylamine and 2.5 parts of di-tert-butyl-p-cresol.
The PAO used in this comparative example was the same as in example 1.
The phenyl silicone oil used in this comparative example was the same as in example 1.
The lithium 12-hydroxystearate and lithium stearate used in this comparative example were the same as in example 1.
The organobentonite used in this comparative example was the same as in example 1.
The comparative example also provides a preparation method of the ultralow temperature lubricating grease, which comprises the following steps: (1) weighing phenyl silicone oil, base oil, a thickening agent and polytetrafluoroethylene powder, heating to 100 ℃, stirring, and reacting for 3 hours; (2) adding lithium hydroxide into the step (1), and then performing saponification reaction at 120 ℃ for 8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 220 ℃ for high-temperature refining, wherein the reaction time is 3 hours, cooling to 100 ℃, finally adding di-tert-butyl-p-cresol and diphenylamine, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease. This grease was designated as D3.
Comparative example 4
Comparative example 4 provides an ultralow temperature lubricating grease, and the raw materials comprise, by weight, 60 parts of phenyl silicone oil (the phenyl silicone oil with the average viscosity of 30 and the phenyl silicone oil with the average viscosity of 75 are compounded in a weight ratio of 3: 2), 90 parts of PAO base oil (the PAO4 and the PAO8 are compounded in a weight ratio of 2: 1), 20 parts of a compound thickener (12-lithium hydroxystearate, lithium stearate and organic bentonite are compounded in a weight ratio of 1: 3: 4), 20 parts of lithium hydroxide, 8 parts of polytetrafluoroethylene powder (polytetrafluoroethylene with the average fineness of 20nm and compounded polytetrafluoroethylene with the average fineness of 50nm are compounded in a weight ratio of 3: 2), 2.5 parts of diphenylamine and 2.5 parts of di-tert-butyl-p-cresol.
The PAO used in this comparative example was the same as in example 1.
The phenyl silicone oil used in this comparative example was the same as in example 1.
The lithium 12-hydroxystearate and lithium stearate used in this comparative example were the same as in example 1.
The organobentonite used in this comparative example was the same as in example 1.
The comparative example also provides a preparation method of the ultralow temperature lubricating grease, which comprises the following steps: (1) weighing phenyl silicone oil, base oil, a thickening agent and polytetrafluoroethylene powder, heating to 100 ℃, stirring, and reacting for 3 hours; (2) adding lithium hydroxide into the step (1), and then performing saponification reaction at 120 ℃ for 8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 220 ℃ for high-temperature refining, wherein the reaction time is 3 hours, cooling to 100 ℃, finally adding di-tert-butyl-p-cresol and diphenylamine, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease. This grease was designated as D4.
Comparative example 5
Comparative example 5 provides an ultralow temperature lubricating grease, and the raw materials comprise, by weight, 60 parts of phenyl silicone oil (the phenyl silicone oil with the average viscosity of 30 and the phenyl silicone oil with the average viscosity of 75 are compounded in a weight ratio of 3: 2), 90 parts of PAO base oil (the PAO4 and the PAO8 are compounded in a weight ratio of 2: 1), 20 parts of a compound thickener (12-lithium hydroxystearate, lithium stearate and organic bentonite are compounded in a weight ratio of 6: 1: 1), 20 parts of lithium hydroxide, 8 parts of polytetrafluoroethylene powder (polytetrafluoroethylene with the average fineness of 20nm and compounded polytetrafluoroethylene with the average fineness of 50nm are compounded in a weight ratio of 3: 2), 2.5 parts of diphenylamine and 2.5 parts of di-tert-butyl-p-cresol.
The PAO used in this comparative example was the same as in example 1.
The phenyl silicone oil used in this comparative example was the same as in example 1.
The lithium 12-hydroxystearate and lithium stearate used in this comparative example were the same as in example 1.
The organobentonite used in this comparative example was the same as in example 1.
The comparative example also provides a preparation method of the ultralow temperature lubricating grease, which comprises the following steps: (1) weighing phenyl silicone oil, base oil, a thickening agent and polytetrafluoroethylene powder, heating to 100 ℃, stirring, and reacting for 3 hours; (2) adding lithium hydroxide into the step (1), and then performing saponification reaction at 120 ℃ for 8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 220 ℃ for high-temperature refining, wherein the reaction time is 3 hours, cooling to 100 ℃, finally adding di-tert-butyl-p-cresol and diphenylamine, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease. This grease was designated as D5.
Comparative example 6
Comparative example 6 provides an ultralow temperature lubricating grease, and the raw materials comprise, by weight, 60 parts of phenyl silicone oil (the phenyl silicone oil with the average viscosity of 30 and the phenyl silicone oil with the average viscosity of 75 are compounded in a weight ratio of 3: 2), 90 parts of PAO base oil (the PAO4 and the PAO8 are compounded in a weight ratio of 2: 1), 20 parts of a compound thickener (12-lithium hydroxystearate, lithium stearate and organic bentonite are compounded in a weight ratio of 1: 1: 2), 20 parts of lithium hydroxide, 8 parts of polytetrafluoroethylene powder (polytetrafluoroethylene with the average fineness of 20nm and compounded polytetrafluoroethylene with the average fineness of 50nm are compounded in a weight ratio of 3: 2), and 2.5 parts of di-tert-butyl-p-cresol.
The PAO used in this comparative example was the same as in example 1.
The phenyl silicone oil used in this comparative example was the same as in example 1.
The lithium 12-hydroxystearate and lithium stearate used in this comparative example were the same as in example 1.
The organobentonite used in this comparative example was the same as in example 1.
The comparative example also provides a preparation method of the ultralow temperature lubricating grease, which comprises the following steps: (1) weighing phenyl silicone oil, base oil, a thickening agent and polytetrafluoroethylene powder, heating to 100 ℃, stirring, and reacting for 3 hours; (2) adding lithium hydroxide into the step (1), and then performing saponification reaction at 120 ℃ for 8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 220 ℃ for high-temperature refining, wherein the reaction time is 3 hours, cooling to 100 ℃, finally adding di-tert-butyl-p-cresol and diphenylamine, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease. This grease was designated as D6.
Comparative example 7
Comparative example 7 provides an ultralow temperature lubricating grease, and the raw materials comprise, by weight, 60 parts of phenyl silicone oil (the phenyl silicone oil with the average viscosity of 30 and the phenyl silicone oil with the average viscosity of 75 are compounded in a weight ratio of 3: 2), 90 parts of PAO base oil (the PAO4 and the PAO8 are compounded in a weight ratio of 2: 1), 20 parts of a compound thickener (12-lithium hydroxystearate, lithium stearate and organic bentonite are compounded in a weight ratio of 1: 1: 2), 20 parts of lithium hydroxide, 8 parts of polytetrafluoroethylene powder (polytetrafluoroethylene with the average fineness of 20nm and compound polytetrafluoroethylene with the average fineness of 50nm are compounded in a weight ratio of 3: 2), and 2.5 parts of diphenylamine.
The PAO used in this comparative example was the same as in example 1.
The phenyl silicone oil used in this comparative example was the same as in example 1.
The lithium 12-hydroxystearate and lithium stearate used in this comparative example were the same as in example 1.
The organobentonite used in this comparative example was the same as in example 1.
The comparative example also provides a preparation method of the ultralow temperature lubricating grease, which comprises the following steps: (1) weighing phenyl silicone oil, base oil, a thickening agent and polytetrafluoroethylene powder, heating to 100 ℃, stirring, and reacting for 3 hours; (2) adding lithium hydroxide into the step (1), and then performing saponification reaction at 120 ℃ for 8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 220 ℃ for high-temperature refining, wherein the reaction time is 3 hours, cooling to 100 ℃, finally adding di-tert-butyl-p-cresol and diphenylamine, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease. This grease was designated as D7.
Comparative example 8
Comparative example 8 provides an ultralow temperature lubricating grease, and the raw materials comprise, by weight, 60 parts of phenyl silicone oil (the phenyl silicone oil with the average viscosity of 30 and the phenyl silicone oil with the average viscosity of 75 are compounded in a weight ratio of 3: 2), 90 parts of PAO base oil (the PAO4 and the PAO8 are compounded in a weight ratio of 2: 1), 20 parts of a compound thickener (12-lithium hydroxystearate, lithium stearate and organic bentonite are compounded in a weight ratio of 1: 1: 2), 20 parts of lithium hydroxide, 8 parts of polytetrafluoroethylene powder (polytetrafluoroethylene with the average fineness of 20nm and polytetrafluoroethylene with the average fineness of 50nm are compounded in a weight ratio of 1: 5), 2.5 parts of diphenylamine and 2.5 parts of di-tert-butyl-p-cresol.
The PAO used in this comparative example was the same as in example 1.
The phenyl silicone oil used in this comparative example was the same as in example 1.
The lithium 12-hydroxystearate and lithium stearate used in this comparative example were the same as in example 1.
The organobentonite used in this comparative example was the same as in example 1.
The comparative example also provides a preparation method of the ultralow temperature lubricating grease, which comprises the following steps: (1) weighing phenyl silicone oil, base oil, a thickening agent and polytetrafluoroethylene powder, heating to 100 ℃, stirring, and reacting for 3 hours; (2) adding lithium hydroxide into the step (1), and then performing saponification reaction at 120 ℃ for 8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 220 ℃ for high-temperature refining, wherein the reaction time is 3 hours, cooling to 100 ℃, finally adding di-tert-butyl-p-cresol and diphenylamine, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease. This grease was designated as D8.
Evaluation of Performance
COD removal rate:
2. oil removal rate:
3. dehydration rate:
TABLE 1
Figure BDA0002706332640000251
The ultralow-temperature lubricating grease provided by the invention has excellent low-temperature resistance, curing degree, softness, low-temperature fluidity and service life, is suitable for popularization and use in the ultralow-temperature lubricating grease field, and has a wide development prospect, as can be known from examples 1 to 6 and comparative examples 1 to 6. Wherein example 1 achieves the best pour point, the lowest low temperature torque and the highest softness and low temperature fluidity with the best raw material weight ratio, viscosity, fineness, etc.
Finally, it should be understood that the above-described embodiments are merely preferred embodiments of the present invention, and not intended to limit the present invention, and any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. An ultralow-temperature lubricating grease is characterized in that: the raw materials comprise, by weight, 60-200 parts of base oil, 50-90 parts of silicone oil, 10-20 parts of a thickening agent, 5-20 parts of a saponification reaction agent, 1-8 parts of an additive and 1-5 parts of an auxiliary additive.
2. The ultralow temperature grease according to claim 1, wherein: the base oil is one or a mixture of PAO4, PAO6, PAO8 and PAO10 in poly-alpha olefin; the silicone oil is at least one of phenyl silicone oil, amino silicone oil, dimethyl silicone oil, vinyl silicone oil and methyl silicone oil; the thickening agent is one or a mixture of lithium soap, organic bentonite, carbon black and silica gel fine powder; the saponification reactant is at least one of lithium hydroxide, potassium hydroxide, sodium hydroxide and calcium hydroxide; the additive is at least one of polytetrafluoroethylene, boron nitride, graphite, metal powder, hexadecanoic acid, tetradecanoic acid and boric acid; the auxiliary additive is at least one of di-tert-butyl-p-cresol, phenyl-alpha-aniline, dialkyl dithiophosphate, diphenylamine and hydroquinone.
3. The ultralow temperature grease according to claim 2, wherein: the base oil is PAO4 and PAO8, and the weight ratio of the PAO4 to the PAO8 is 2: 1.
4. the ultralow temperature grease according to claim 3, wherein: the silicone oil is phenyl silicone oil, and the weight ratio of the phenyl silicone oil to the base oil is (1-3): (2-4).
5. The ultralow temperature grease according to claim 4, wherein: the phenyl silicone oil is phenyl silicone oil with average viscosity of 30 and phenyl silicone oil with average viscosity of 75.
6. The ultralow temperature grease according to claim 5, wherein: the weight ratio of the phenyl silicone oil with the average viscosity of 30 to the phenyl silicone oil with the average viscosity of 75 is (2-4): (1-3).
7. The ultralow temperature grease according to claim 6, wherein: the thickening agent is 12-lithium hydroxystearate, lithium stearate and organic bentonite, and the weight ratio of the 12-lithium hydroxystearate to the lithium stearate to the organic bentonite is (1-3): (1-3): (1-3).
8. The ultralow temperature grease according to claim 7, wherein: the additive is polytetrafluoroethylene with the average fineness of 20nm and polytetrafluoroethylene with the average fineness of 50nm, and the weight ratio of the polytetrafluoroethylene with the average fineness of 20nm to the polytetrafluoroethylene with the average fineness of 50nm is (1-3): (1-2).
9. The ultralow temperature grease according to claim 8, wherein: the auxiliary additive is di-tert-butyl-p-cresol and diphenylamine, and the weight ratio of the di-tert-butyl-p-cresol to the diphenol is 1: 1.
10. the method for preparing the ultralow-temperature lubricating grease according to any one of claims 1 to 9, which is characterized by comprising the following steps: (1) weighing base oil, silicone oil, a thickening agent and an additive, heating to 50-120 ℃, stirring, and reacting for 1-3 hours; (2) adding a saponification reactant into the step (1), and then performing saponification reaction at the temperature of 100 ℃ and 130 ℃ for 4-8 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 180-220 ℃ for high-temperature refining, wherein the reaction time is 2.5-5 hours, cooling to 100 ℃, finally adding an auxiliary additive, and homogenizing, degassing and filtering to obtain the ultralow-temperature lubricating grease.
CN202011040005.9A 2020-09-28 2020-09-28 Ultralow-temperature lubricating grease and preparation method thereof Active CN112111313B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011040005.9A CN112111313B (en) 2020-09-28 2020-09-28 Ultralow-temperature lubricating grease and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011040005.9A CN112111313B (en) 2020-09-28 2020-09-28 Ultralow-temperature lubricating grease and preparation method thereof

Publications (2)

Publication Number Publication Date
CN112111313A true CN112111313A (en) 2020-12-22
CN112111313B CN112111313B (en) 2022-05-13

Family

ID=73798644

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011040005.9A Active CN112111313B (en) 2020-09-28 2020-09-28 Ultralow-temperature lubricating grease and preparation method thereof

Country Status (1)

Country Link
CN (1) CN112111313B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114703004A (en) * 2022-04-28 2022-07-05 中国石油化工股份有限公司 Lithium-based lubricating grease composition and preparation method thereof

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4755310A (en) * 1986-06-02 1988-07-05 Shin-Etsu Chemical Co., Ltd. Silicone grease composition containing a chlorinated alicyclic compound
CN1715377A (en) * 2004-06-29 2006-01-04 中国石油化工股份有限公司 Airplane wheel grease and its preparing method
CN101792689A (en) * 2010-02-03 2010-08-04 上海禾泰特种润滑技术有限公司 High-performance complex lithium-calcium base grease composition and method for preparing same
CN102510895A (en) * 2009-10-23 2012-06-20 三菱重工业株式会社 Lubricating oil composition for die forging and die forging device
CN103525510A (en) * 2013-10-15 2014-01-22 中国石油化工股份有限公司 Low-temperature lubricating grease and preparation method thereof
CN104371796A (en) * 2014-10-25 2015-02-25 中国石油化工股份有限公司 Low-temperature lubricating grease composition and preparation method thereof
CN104830406A (en) * 2015-05-14 2015-08-12 新乡市恒星化工有限责任公司 Special lubricating grease for Raymond mill and preparation method of special lubricating grease
CN105087107A (en) * 2015-08-31 2015-11-25 宁夏宝塔石化科技实业发展有限公司 Preparation method of bearing lubricating grease
CN111100724A (en) * 2018-10-25 2020-05-05 中国石油化工股份有限公司 Perfluoropolyether lubricating grease and preparation method thereof

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4755310A (en) * 1986-06-02 1988-07-05 Shin-Etsu Chemical Co., Ltd. Silicone grease composition containing a chlorinated alicyclic compound
CN1715377A (en) * 2004-06-29 2006-01-04 中国石油化工股份有限公司 Airplane wheel grease and its preparing method
CN102510895A (en) * 2009-10-23 2012-06-20 三菱重工业株式会社 Lubricating oil composition for die forging and die forging device
CN101792689A (en) * 2010-02-03 2010-08-04 上海禾泰特种润滑技术有限公司 High-performance complex lithium-calcium base grease composition and method for preparing same
CN103525510A (en) * 2013-10-15 2014-01-22 中国石油化工股份有限公司 Low-temperature lubricating grease and preparation method thereof
CN104371796A (en) * 2014-10-25 2015-02-25 中国石油化工股份有限公司 Low-temperature lubricating grease composition and preparation method thereof
CN104830406A (en) * 2015-05-14 2015-08-12 新乡市恒星化工有限责任公司 Special lubricating grease for Raymond mill and preparation method of special lubricating grease
CN105087107A (en) * 2015-08-31 2015-11-25 宁夏宝塔石化科技实业发展有限公司 Preparation method of bearing lubricating grease
CN111100724A (en) * 2018-10-25 2020-05-05 中国石油化工股份有限公司 Perfluoropolyether lubricating grease and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114703004A (en) * 2022-04-28 2022-07-05 中国石油化工股份有限公司 Lithium-based lubricating grease composition and preparation method thereof

Also Published As

Publication number Publication date
CN112111313B (en) 2022-05-13

Similar Documents

Publication Publication Date Title
CN102277224B (en) Lubricant composition for transmission system of wind power equipment
CN101921652A (en) Oil-air lubricating grease and production method thereof
KR20110031482A (en) Grease composition
CN106701290B (en) Lubricating grease composition and preparation method thereof
WO2010037746A1 (en) Grease composition
CN106010754A (en) Compressor oil composition containing trimethylol propane ester
CN102031186B (en) Expanding oil and preparation method thereof
CN112111313B (en) Ultralow-temperature lubricating grease and preparation method thereof
CN107987927B (en) Steel wire rope oil composition
WO2007066636A1 (en) Grease composition and bearing
CN108865339B (en) Lubricating grease composition for axle box bearing of high-speed motor train unit and preparation method thereof
JP5411457B2 (en) Lubricant composition
CN102337176A (en) Hydraulic oil composition with low viscosity and low solidifying point
CN109233980B (en) Lubricating grease and preparation method thereof
JP2016121336A (en) Grease composition
JPH04266995A (en) Grease composition for speed reducer
CN115058270B (en) Degradable wheel rail antifriction film forming paste and preparation method thereof
CN105038932A (en) Lubricating oil and preparation method thereof
CN112812874B (en) Lubricating grease for aviation high-temperature motor bearing
JP5765806B2 (en) Grease composition
CN109504515B (en) Energy-saving environment-friendly agricultural machine oil and preparation method thereof
CN114517118B (en) Graphite alkyne lubricating oil composition and preparation method thereof
JPH01229096A (en) Dispersant for solid lubricant
CN101993768B (en) Multifunctional lubricating grease and preparation method thereof
CN104277895A (en) Chain lubricating oil and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant