CN112048354A - Long-acting high-temperature lubricating grease and preparation method thereof - Google Patents

Long-acting high-temperature lubricating grease and preparation method thereof Download PDF

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Publication number
CN112048354A
CN112048354A CN202011006087.5A CN202011006087A CN112048354A CN 112048354 A CN112048354 A CN 112048354A CN 202011006087 A CN202011006087 A CN 202011006087A CN 112048354 A CN112048354 A CN 112048354A
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parts
long
lubricating grease
grease
modified carbon
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高巍
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Harbin Sino Japanese Oil Chemical Industry Co ltd
Shanghai Hutou Chemical Co ltd
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Harbin Sino Japanese Oil Chemical Industry Co ltd
Shanghai Hutou Chemical Co ltd
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Priority to CN202011006087.5A priority Critical patent/CN112048354A/en
Publication of CN112048354A publication Critical patent/CN112048354A/en
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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
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/168—After-treatment
    • 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
    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/02—Carbon; Graphite
    • 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
    • C10M2201/04—Elements
    • C10M2201/041—Carbon; Graphite; Carbon black
    • 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
    • C10M2201/061—Carbides; Hydrides; Nitrides
    • 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
    • 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
    • C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
    • 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
    • C10M2207/024—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings having at least two phenol groups but no condensed ring
    • 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]
    • C10M2213/0626—Polytetrafluoroethylene [PTFE] 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
    • 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
    • C10M2229/041—Siloxanes with specific structure containing aliphatic substituents
    • C10M2229/0415—Siloxanes with specific structure containing aliphatic substituents used as base material

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Lubricants (AREA)

Abstract

The invention discloses long-acting high-temperature lubricating grease which comprises, by weight, 70-200 parts of base oil, 10-20 parts of a thickening agent, 1-5 parts of modified carbon nanotubes, 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 high-viscosity dimethyl silicone oil, the thickening agent is polytetrafluoroethylene, and the modified carbon nano tube is a polyazole modified carbon nano tube. According to the invention, through the restriction on the viscosity of the base oil, the modification and addition of the carbon nano tubes, the fineness restriction of the thickening agent and the compounding of various additives, the prepared lubricating grease has excellent dropping point, softness and high-temperature thermal stability, can be effectively used for a long time, is suitable for being popularized and used as a long-acting high-temperature lubricating grease in the field of lubricating grease, and has a wide development prospect.

Description

Long-acting high-temperature lubricating grease and preparation method thereof
Technical Field
The invention relates to the field of lubricating grease, in particular to long-acting high-temperature lubricating grease and a preparation method thereof.
Background
Compared with the existing lubricating oil, the lubricating grease serving as a common lubricating medium has the characteristics of excellent stability, oxidation resistance, mechanical stability, adhesion, extreme pressure wear resistance, sealing property and the like, and is suitable for being applied to lubricating parts of mechanical equipment with higher requirements on motion precision, bearing capacity, extreme pressure property, rotating speed and service life. With the continuous development of industrial modernization, the parts needing lubrication, such as mechanical equipment and the like, have higher and higher requirements on the use temperature resistance of the lubricating grease. Most of the existing high-temperature lubricating grease has the actions of softening, oil separation, drying cracking, melting, volatilization, hardening and the like under the high-temperature condition, and the phenomena cause the lubricating grease to lose the lubricating effect, so that mechanical equipment is damaged by abrasion, sintering, seizure and the like, and the mechanical equipment cannot work, is maintained in a large quantity, has a reduced service life and the like.
In the process of implementing the technical scheme of the invention in the embodiment of the present application, the inventor of the present application finds that at least the following technical problems exist in the prior art:
for example, the invention patent with the publication number of CN104560290B discloses a composite barium-based lubricating grease and a preparation method thereof. Based on the weight of the lubricating grease, the composite barium-based lubricating grease comprises the following components: 65-95% of lubricating base oil, 5-30% of composite barium-based thickening agent and 0.2-15% of graphene, wherein the decomposition temperature reaches 430-480 ℃, but decomposition and large cracking residue still occur in an environment above 450 ℃, and the working life at high temperature and the ultra-high temperature resistance and antirust capacity are improved.
The invention realizes a long-acting high-temperature lubricating oil which still shows good lubricating effect under high temperature and has good dropping point, corrosion inhibition, softness and excellent thermal stability after long-time work.
Disclosure of Invention
In order to solve the problems, the first aspect of the invention provides long-acting high-temperature lubricating grease, which comprises, by weight, 70-200 parts of base oil, 10-20 parts of a thickening agent, 1-5 parts of modified carbon nanotubes, 5-20 parts of a saponification reaction agent, 1-8 parts of an additive and 1-5 parts of an auxiliary additive.
As a preferable scheme, the base oil is at least one of dimethyl silicone oil, ethyl silicone oil, phenyl silicone oil, methyl hydrogen-containing silicone oil, methyl phenyl silicone oil, methyl chlorphenyl silicone oil and cycloalkyl rubber silicone oil; the thickening agent is at least one of polytetrafluoroethylene, composite calcium sulfonate, composite lithium, composite aluminum, bentonite, polyurea and polyethylene; the saponification reactant is at least one of sodium hydroxide, potassium hydroxide, calcium hydroxide, lithium hydroxide and concentrated ammonia water; the additive is at least one of boron nitride, graphite, metal powder, stearic acid and boric acid; the auxiliary additive is at least one of diphenylamine, ethylene diamine tetraacetic acid tetrabenzyl amide, hydroquinone, thiobisphenol and triphenol.
Preferably, the base oil is dimethicone with average viscosity of 400-600, and dimethicone with average viscosity of 700-1000.
Preferably, the weight ratio of the simethicone with the average viscosity of 400-600 to the simethicone with the average viscosity of 700-1000 is (1-3): (2-4).
Preferably, the modified carbon nanotube is a polyazole modified carbon nanotube.
As a preferable scheme, the weight ratio of the modified carbon nanotubes to the base oil is 1: (40-200).
In a preferred embodiment, the thickener is PTFE with an average fineness of 40nm, PTFE with an average fineness of 80nm and PTFE with an average fineness of 120 nm.
Preferably, the PTFE with the average fineness of 40nm and the weight ratio of the PTFE with the average fineness of 80nm to the PTFE with the average fineness of 120nm are (1-3): (1-3): (1-3).
In a preferred embodiment, the auxiliary additives are diphenylamine and hydroquinone.
The second aspect of the invention provides a preparation method of long-acting high-temperature lubricating grease, which comprises the following steps: (1) weighing the base oil, the thickening agent, the modified carbon nano tube and the 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 long-acting high-temperature lubricating grease.
Has the advantages that: the invention provides long-acting high-temperature lubricating grease and a preparation method thereof, and the prepared lubricating grease has excellent dropping point, softness and high-temperature thermal stability, can be effectively used for a long time, is suitable for being popularized and used as long-acting high-temperature lubricating grease in the field of lubricating grease and has wide development prospect by various modes of limiting the viscosity of base oil, modifying and adding carbon nano tubes, limiting the fineness of a thickening agent and compounding various additives.
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 first aspect of the invention provides long-acting high-temperature lubricating grease, which comprises, by weight, 70-200 parts of base oil, 10-20 parts of a thickening agent, 1-5 parts of modified carbon nanotubes, 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 at least one of dimethyl silicone oil, ethyl silicone oil, phenyl silicone oil, methyl hydrogen silicone oil, methyl phenyl silicone oil, methyl chlorophenyl silicone oil, and cycloalkyl rubber silicone oil; the thickening agent is at least one of polytetrafluoroethylene, composite calcium sulfonate, composite lithium, composite aluminum, bentonite, polyurea and polyethylene; the saponification reactant is at least one of sodium hydroxide, potassium hydroxide, calcium hydroxide, lithium hydroxide and concentrated ammonia water; the additive is at least one of boron nitride, graphite, metal powder, stearic acid and boric acid; the auxiliary additive is at least one of diphenylamine, ethylene diamine tetraacetic acid tetrabenzyl amide, hydroquinone, thiobisphenol and triphenol.
The saponification reagent is an essential reagent for saponification, and usually a strong alkaline solution reacts with an ester-based substance to obtain alcohol, carboxylate and glycerol, which are key steps for preparing soap and grease. The alkaline solutions generally used are sodium hydroxide and potassium hydroxide, and the saponification number is defined as the number of milligrams of potassium hydroxide consumed by the alkaline hydrolysis of 1g of fats and oils.
In some preferred embodiments, the base oil is a dimethicone having an average viscosity of 400 to 600 and a dimethicone having an average viscosity of 700 to 1000.
In some preferred embodiments, the weight ratio of the simethicone with the average viscosity of 400-600 to the simethicone with the average viscosity of 700-1000 is (1-3): (2-4). When the dimethyl silicone oil compounded by the dimethyl silicone oil with the average viscosity of 400-600 and the dimethyl silicone oil with the average viscosity of 700-1000 is used as the base oil, the thermal stability of the lubricating grease and the temperature of liquid state transition and dripping of the lubricating grease are improved. The applicant speculates that the reason is that different powder-eating capacities of the dimethyl silicone oil with different viscosities act on the thickening agent powder with different fineness to have better filling effect, so that the thickening agent achieves better medium filling and skeleton structure effects.
The viscosity unit in this application is cSt, the name centistokes, and is a kinematic viscosity unit representing the ratio of the dynamic viscosity of a fluid to the density of the fluid at the same temperature, and in International units (SI), the kinematic viscosity unit is m2/s，1cSt＝10-6m2/s＝1mm2The amount/s can be measured according to the method described in GB/T256-88 or ASTM D445-96.
The dimethylsilicone fluids used in the present application are commercially available, for example, QL-200DM 500 and QL-200DM 1000, available from Strength chemical industries, Ltd.
In some preferred embodiments, the modified carbon nanotubes are polyacene-modified carbon nanotubes.
The addition of the polynitrogen cyclopentadiene modified carbon nano tube improves the liquid transition dropping temperature, the thermal stability and the metal protection property of the lubricating grease. The N element rich in the polynitrogen modified carbon nano tube improves the heat resistance of the lubricating grease. Meanwhile, the polynitrogen metallocene has passivation and shielding effects on metal, the metal potential is improved, the phenomenon of losing electrons of metal surface atoms is greatly slowed down under the synergistic effect of the polynitrogen metallocene and a compound auxiliary additive, and the carbon nano tube has stronger structural rigidity and better heat resistance and oxygen resistance, so that the thermal stability and the service life of the lubricating grease can be improved after the carbon nano tube is introduced.
The polynitrogen cyclopentadiene modified carbon nano tube is self-made, and comprises the following steps: (1) adding a certain amount of nitrogen metallocene and multi-wall carbon nano-tubes into 500mL of H at the same time2SO4In the solution (0.1mol/L), ultrasonic dispersion is carried out for 2 hours, and a mixed solution with complete dispersion is obtained. (2) Dropwise adding 200mL FeCl into the mixed solution under the protection of nitrogen atmosphere and ice bath3And continuously stirring the solution for reaction for 8 hours, centrifugally washing and drying in vacuum after the reaction is finished, and grinding and sieving to obtain the powdery polyazole modified carbon nano tube.
The multi-walled carbon nanotubes in the present application can be commercially available products such as multi-walled carbon nanotubes, hydroxyl multi-walled carbon nanotubes, carboxyl multi-walled carbon nanotubes, and the like, which are manufactured by the Ishikaki technologies, Inc. of Beijing Deke.
The metallocenes (CAS number 109-97-7) in the present application may be commercially available, for example, the P0574 metallocene product produced by Shanghai Chiloeichen chemical industry Co., Ltd.
In some preferred embodiments, the weight ratio of the modified carbon nanotubes to the base oil is 1: (40-200). The proper amount of the added polyacene modified carbon nano-tube is beneficial to improving the overall performance of the lubricating grease at high temperature. The applicant speculates that stronger interfacial force is generated between the cladding structure and hydrophilic groups (such as carboxyl and hydroxyl) on the surface of the polyacene modified carbon nano tube and a base oil body, so that the compatibility and affinity among all substances of the lubricating grease system are promoted, and the whole dispersibility of the lubricating grease system is higher. When the addition amount of the polyacene modified carbon nano tube is less than 1: (40-200), too little addition of the polyacene modified carbon nanotube is not favorable for the polyacene modified carbon nanotube to function in the grease, and thus various properties of the grease cannot be effectively improved. When the addition amount of the polyacene modified carbon nano tube is more than 1: (40 to 200), the amount of the polyacene modified carbon nanotubes added is too large, and although the advantageous effects of the polyacene modified carbon nanotubes can be exerted, the too large amount of the polyacene modified carbon nanotubes affects other properties of the grease, such as the overall kinematic viscosity of the grease, the softness of the grease, and the lubricating effect and wear resistance of the grease.
In some preferred embodiments, the thickener is PTFE with an average fineness of 40nm, PTFE with an average fineness of 80nm and PTFE with an average fineness of 120 nm.
In some preferred embodiments, the weight ratio of PTFE with an average fineness of 40nm, PTFE with an average fineness of 80nm and PTFE with an average fineness of 120nm is (1-3): (1-3): (1-3).
Polytetrafluoroethylene (CAS number: 9002-84-0) (PTFE) is commonly called "Plastic King", and is a high molecular polymer. Presents white wax-like appearance, has excellent heat resistance and cold resistance, and can be used for a long time at the temperature of minus 180-300 ℃. PTFE has excellent chemical stability, corrosion resistance, sealing property and ageing resistance, is the lowest friction coefficient of solid materials, and is an excellent lubricating grease thickening agent.
The fineness of the material is 40nm, 80nm and 120nm according to the weight ratio (1-3): (1-3): (1-3) the polytetrafluoroethylene powder prepared by compounding is used as a thickening agent, so that the curing degree and the heat resistance of the lubricating grease are improved. Presumably, the following: the polytetrafluoroethylene compounded with the fineness can be quickly filled in the compounded silicone oil, does not generate precipitation and aggregation, and does not need an additional oleophilic type suspension forming agent, so that other properties of the lubricating grease can not be influenced.
In some preferred embodiments, the supplemental additives are diphenylamine (CAS number: 122-39-4) and hydroquinone (CAS number: 123-31-9).
In some preferred embodiments, the supplemental additives are diphenylamine and hydroquinone in a ratio of 1: 1 weight ratio. The diphenylamine and the hydroquinone which are compounded are added into the lubricating grease together for a synergistic effect, and the compounding of the amine and the phenol has a more obvious effect on reducing the electron loss phenomenon of the atoms in the lubricating grease than the use of a single kind. Phenols and amines as radical scavengers can trap active free agents, change the active free agents into inactive substances, inhibit continuous electron-losing reactions, and the phenols contribute to the regeneration of the amines, and the synergistic effect of the phenols and the amines with the polyazole-modified carbon nanotubes greatly improves the thermal stability of the grease.
The second aspect of the present invention provides a method for preparing the long-acting high-temperature grease, comprising the following steps: (1) weighing the base oil, the thickening agent, the modified carbon nano tube and the 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 long-acting high-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 a long-acting high-temperature lubricating grease, which comprises the following raw materials, by weight, 200 parts of simethicone (with an average kinematic viscosity of 500, compounded at a weight ratio of 2: 3 to 1000), 20 parts of polytetrafluoroethylene powder (with an average fineness of 40nm, 80nm, compounded at a weight ratio of 1: 2: 3 to 120 nm), 5 parts of a polyazole modified carbon nanotube, 20 parts of sodium hydroxide, 8 parts of boron nitride, 2.5 parts of diphenylamine and 2.5 parts of hydroquinone.
The dimethyl silicone oil in the embodiment is QL-200DM 500 and QL-200DM 1000 products produced by Strength chemical engineering Co., Ltd.
The polynitrogen modified carbon nano tube in the embodiment is self-made, and the steps are as follows: (1) 5g of metallocene, 2.5g of multiwall carbon nanotubes were added simultaneously to 250mL of H2SO4In the aqueous solution (0.1mol/L), ultrasonic dispersion is carried out for 2 hours, and a mixed solution with complete dispersion is obtained. (2) Dropwise adding 100mL of 1mol/L FeCl into the mixed solution under the protection of nitrogen atmosphere and ice bath (0℃)3And (3) continuously stirring the aqueous solution for reacting for 8 hours, then centrifugally washing, drying in vacuum, and grinding and sieving to obtain the powdery polyazole modified carbon nano tube.
The multi-walled carbon nanotube in this embodiment is a hydroxyl multi-walled carbon nanotube product produced by dekojijin technologies ltd, beijing.
The metallocenes in this example are P0574 products produced by Daihei chemical industry Limited, Shanghai.
The embodiment also provides a preparation method of the long-acting high-temperature lubricating grease, which comprises the following steps: (1) weighing dimethyl silicone oil, polytetrafluoroethylene powder, a polybenzazole modified carbon nano tube and boron nitride, heating to 120 ℃, stirring and reacting for 3 hours; (2) adding sodium hydroxide into the step (1), and then performing saponification reaction at 130 ℃ for 6 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 200 ℃ for high-temperature refining, wherein the reaction time is 4 hours, cooling to 100 ℃, finally adding diphenylamine and hydroquinone, and homogenizing, degassing and filtering to obtain the long-acting high-temperature lubricating grease. This grease was designated as R1.
Example 2
Embodiment 2 provides a long-acting high-temperature lubricating grease, which comprises the following raw materials, by weight, 200 parts of simethicone (with an average kinematic viscosity of 500, compounded at a weight ratio of 1: 4 to 1000), 20 parts of polytetrafluoroethylene powder (with an average fineness of 40nm, 80nm, compounded at a weight ratio of 1: 2: 3 to 120 nm), 5 parts of a polyazole modified carbon nanotube, 20 parts of sodium hydroxide, 8 parts of boron nitride, 2.5 parts of diphenylamine and 2.5 parts of hydroquinone.
The dimethylsilicone oil used in this example was the same as in example 1.
The polyacene-modified carbon nanotubes used in this example were the same as those used in example 1.
The multi-walled carbon nanotubes used in this example were the same as in example 1.
The metallocenes used in this example were the same as in example 1.
The embodiment also provides a preparation method of the long-acting high-temperature lubricating grease, which comprises the following steps: (1) weighing dimethyl silicone oil, polytetrafluoroethylene powder, a polybenzazole modified carbon nano tube and boron nitride, heating to 120 ℃, stirring and reacting for 3 hours; (2) adding sodium hydroxide into the step (1), and then performing saponification reaction at 130 ℃ for 6 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 200 ℃ for high-temperature refining, wherein the reaction time is 4 hours, cooling to 100 ℃, finally adding diphenylamine and hydroquinone, and homogenizing, degassing and filtering to obtain the long-acting high-temperature lubricating grease. This grease was designated as R2.
Example 3
Embodiment 3 provides a long-acting high-temperature lubricating grease, which comprises the following raw materials, by weight, 200 parts of simethicone (with an average kinematic viscosity of 500, compounded at a weight ratio of 3: 2 for 1000), 20 parts of polytetrafluoroethylene powder (with an average fineness of 40nm, 80nm, compounded at a weight ratio of 1: 2: 3 for 120 nm), 5 parts of a polyazole modified carbon nanotube, 20 parts of sodium hydroxide, 8 parts of boron nitride, 2.5 parts of diphenylamine, and 2.5 parts of hydroquinone.
The dimethylsilicone oil used in this example was the same as in example 1.
The polyacene-modified carbon nanotubes used in this example were the same as those used in example 1.
The multi-walled carbon nanotubes used in this example were the same as in example 1.
The metallocenes used in this example were the same as in example 1.
The embodiment also provides a preparation method of the long-acting high-temperature lubricating grease, which comprises the following steps: (1) weighing dimethyl silicone oil, polytetrafluoroethylene powder, a polybenzazole modified carbon nano tube and boron nitride, heating to 120 ℃, stirring and reacting for 3 hours; (2) adding sodium hydroxide into the step (1), and then performing saponification reaction at 130 ℃ for 6 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 200 ℃ for high-temperature refining, wherein the reaction time is 4 hours, cooling to 100 ℃, finally adding diphenylamine and hydroquinone, and homogenizing, degassing and filtering to obtain the long-acting high-temperature lubricating grease. This grease was designated as R3.
Example 4
Embodiment 4 provides a long-acting high-temperature lubricating grease, which comprises, by weight, 200 parts of dimethicone (average kinematic viscosity 500, 1000 compounded in a weight ratio of 2: 3), 20 parts of polytetrafluoroethylene powder (average fineness 40nm, 80nm, 120nm compounded in a weight ratio of 1: 1: 1), 5 parts of a polyazole modified carbon nanotube, 20 parts of sodium hydroxide, 8 parts of boron nitride, 2.5 parts of diphenylamine, and 2.5 parts of hydroquinone.
The dimethylsilicone oil used in this example was the same as in example 1.
The polyacene-modified carbon nanotubes used in this example were the same as those used in example 1.
The multi-walled carbon nanotubes used in this example were the same as in example 1.
The metallocenes used in this example were the same as in example 1.
The embodiment also provides a preparation method of the long-acting high-temperature lubricating grease, which comprises the following steps: (1) weighing dimethyl silicone oil, polytetrafluoroethylene powder, a polybenzazole modified carbon nano tube and boron nitride, heating to 120 ℃, stirring and reacting for 3 hours; (2) adding sodium hydroxide into the step (1), and then performing saponification reaction at 130 ℃ for 6 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 200 ℃ for high-temperature refining, wherein the reaction time is 4 hours, cooling to 100 ℃, finally adding diphenylamine and hydroquinone, and homogenizing, degassing and filtering to obtain the long-acting high-temperature lubricating grease. This grease was designated as R4.
Example 5
Embodiment 5 provides a long-acting high-temperature lubricating grease, which comprises the following raw materials, by weight, 200 parts of simethicone (with an average kinematic viscosity of 500, compounded at a weight ratio of 2: 3 to 1000), 20 parts of polytetrafluoroethylene powder (with an average fineness of 40nm, 80nm, compounded at a weight ratio of 3: 2: 1 to 120 nm), 5 parts of a polyazole modified carbon nanotube, 20 parts of sodium hydroxide, 8 parts of boron nitride, 2.5 parts of diphenylamine, and 2.5 parts of hydroquinone.
The dimethylsilicone oil used in this example was the same as in example 1.
The polyacene-modified carbon nanotubes used in this example were the same as those used in example 1.
The multi-walled carbon nanotubes used in this example were the same as in example 1.
The metallocenes used in this example were the same as in example 1.
The embodiment also provides a preparation method of the long-acting high-temperature lubricating grease, which comprises the following steps: (1) weighing dimethyl silicone oil, polytetrafluoroethylene powder, a polybenzazole modified carbon nano tube and boron nitride, heating to 120 ℃, stirring and reacting for 3 hours; (2) adding sodium hydroxide into the step (1), and then performing saponification reaction at 130 ℃ for 6 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 200 ℃ for high-temperature refining, wherein the reaction time is 4 hours, cooling to 100 ℃, finally adding diphenylamine and hydroquinone, and homogenizing, degassing and filtering to obtain the long-acting high-temperature lubricating grease. This grease was designated as R5.
Example 6
Embodiment 6 provides a long-acting high-temperature lubricating grease, which comprises the following raw materials, by weight, 200 parts of simethicone (with an average kinematic viscosity of 500, compounded at a weight ratio of 2: 2 of 1000), 20 parts of polytetrafluoroethylene powder (with an average fineness of 40nm, 80nm, compounded at a weight ratio of 1: 2: 1 of 120 nm), 5 parts of a polyazole modified carbon nanotube, 20 parts of sodium hydroxide, 8 parts of boron nitride, 2.5 parts of diphenylamine, and 2.5 parts of hydroquinone.
The dimethylsilicone oil used in this example was the same as in example 1.
The polyacene-modified carbon nanotubes used in this example were the same as those used in example 1.
The multi-walled carbon nanotubes used in this example were the same as in example 1.
The metallocenes used in this example were the same as in example 1.
The embodiment also provides a preparation method of the long-acting high-temperature lubricating grease, which comprises the following steps: (1) weighing dimethyl silicone oil, polytetrafluoroethylene powder, a polybenzazole modified carbon nano tube and boron nitride, heating to 120 ℃, stirring and reacting for 3 hours; (2) adding sodium hydroxide into the step (1), and then performing saponification reaction at 130 ℃ for 6 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 200 ℃ for high-temperature refining, wherein the reaction time is 4 hours, cooling to 100 ℃, finally adding diphenylamine and hydroquinone, and homogenizing, degassing and filtering to obtain the long-acting high-temperature lubricating grease. This grease was designated as R6.
Example 7
Embodiment 7 provides a long-acting high-temperature lubricating grease, which comprises the following raw materials, by weight, 200 parts of simethicone (with an average kinematic viscosity of 500, compounded at a weight ratio of 2: 3 to 1000), 20 parts of polytetrafluoroethylene powder (with an average fineness of 40nm, 80nm, compounded at a weight ratio of 1: 2: 3 to 120 nm), 1 part of a polyazole modified carbon nanotube, 20 parts of sodium hydroxide, 8 parts of boron nitride, 2.5 parts of diphenylamine, and 2.5 parts of hydroquinone.
The dimethylsilicone oil used in this example was the same as in example 1.
The polyacene-modified carbon nanotubes used in this example were the same as those used in example 1.
The multi-walled carbon nanotubes used in this example were the same as in example 1.
The metallocenes used in this example were the same as in example 1.
The embodiment also provides a preparation method of the long-acting high-temperature lubricating grease, which comprises the following steps: (1) weighing dimethyl silicone oil, polytetrafluoroethylene powder, a polybenzazole modified carbon nano tube and boron nitride, heating to 120 ℃, stirring and reacting for 3 hours; (2) adding sodium hydroxide into the step (1), and then performing saponification reaction at 130 ℃ for 6 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 200 ℃ for high-temperature refining, wherein the reaction time is 4 hours, cooling to 100 ℃, finally adding diphenylamine and hydroquinone, and homogenizing, degassing and filtering to obtain the long-acting high-temperature lubricating grease. This grease was designated as R7.
Example 8
Embodiment 8 provides a long-acting high-temperature lubricating grease, which comprises the following raw materials, by weight, 200 parts of simethicone (with an average kinematic viscosity of 500, compounded at a weight ratio of 2: 3 to 1000), 20 parts of polytetrafluoroethylene powder (with an average fineness of 40nm, 80nm, compounded at a weight ratio of 1: 2: 3 to 120 nm), 2.5 parts of a polyazole modified carbon nanotube, 20 parts of sodium hydroxide, 8 parts of boron nitride, 2.5 parts of diphenylamine, and 2.5 parts of hydroquinone.
The dimethylsilicone oil used in this example was the same as in example 1.
The polyacene-modified carbon nanotubes used in this example were the same as those used in example 1.
The multi-walled carbon nanotubes used in this example were the same as in example 1.
The metallocenes used in this example were the same as in example 1.
The embodiment also provides a preparation method of the long-acting high-temperature lubricating grease, which comprises the following steps: (1) weighing dimethyl silicone oil, polytetrafluoroethylene powder, a polybenzazole modified carbon nano tube and boron nitride, heating to 120 ℃, stirring and reacting for 3 hours; (2) adding sodium hydroxide into the step (1), and then performing saponification reaction at 130 ℃ for 6 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 200 ℃ for high-temperature refining, wherein the reaction time is 4 hours, cooling to 100 ℃, finally adding diphenylamine and hydroquinone, and homogenizing, degassing and filtering to obtain the long-acting high-temperature lubricating grease. This grease was designated as R8.
Comparative example 1
Comparative example 1 provides a long-acting high-temperature lubricating grease, and the raw materials comprise, by weight, 200 parts of dimethicone (average kinematic viscosity 500, 1000 compounded in a weight ratio of 5: 1), 20 parts of polytetrafluoroethylene powder (average fineness 40nm, 80nm, 120nm compounded in a weight ratio of 1: 2: 3), 5 parts of polyazole modified carbon nanotube, 20 parts of sodium hydroxide, 8 parts of boron nitride, 2.5 parts of diphenylamine, and 2.5 parts of hydroquinone.
The dimethylsilicone oil used in this comparative example was the same as in example 1.
The polyacene modified carbon nanotubes used in this comparative example were the same as in example 1.
The multi-walled carbon nanotubes used in this comparative example were the same as in example 1.
The metallocene used in this comparative example was the same as in example 1.
The comparative example also provides a method for preparing the long-acting high-temperature lubricating grease: (1) weighing dimethyl silicone oil, polytetrafluoroethylene powder, a polybenzazole modified carbon nano tube and boron nitride, heating to 120 ℃, stirring and reacting for 3 hours; (2) adding sodium hydroxide into the step (1), and then performing saponification reaction at 130 ℃ for 6 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 200 ℃ for high-temperature refining, wherein the reaction time is 4 hours, cooling to 100 ℃, finally adding diphenylamine and hydroquinone, and homogenizing, degassing and filtering to obtain the long-acting high-temperature lubricating grease. This grease was designated as D1.
Comparative example 2
Comparative example 2 provides a long-acting high-temperature lubricating grease, and the raw materials comprise, by weight, 200 parts of dimethicone (average kinematic viscosity 500, 1000 compounded in a weight ratio of 2: 3), 20 parts of polytetrafluoroethylene powder (average fineness 40nm, 80nm, 120nm compounded in a weight ratio of 1: 2: 3), 5 parts of multi-walled carbon nanotubes, 20 parts of sodium hydroxide, 8 parts of boron nitride, 2.5 parts of diphenylamine, and 2.5 parts of hydroquinone.
The dimethylsilicone oil used in this comparative example was the same as in example 1.
The multi-walled carbon nanotubes used in this comparative example were the same as in example 1.
The comparative example also provides a method for preparing the long-acting high-temperature lubricating grease: (1) weighing dimethyl silicone oil, polytetrafluoroethylene powder, multi-walled carbon nanotubes and boron nitride, heating to 120 ℃, stirring, and reacting for 3 hours; (2) adding sodium hydroxide into the step (1), and then performing saponification reaction at 130 ℃ for 6 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 200 ℃ for high-temperature refining, wherein the reaction time is 4 hours, cooling to 100 ℃, finally adding diphenylamine and hydroquinone, and homogenizing, degassing and filtering to obtain the long-acting high-temperature lubricating grease. This grease was designated as D2.
Comparative example 3
Comparative example 3 provides a long-acting high-temperature lubricating grease, which comprises the following raw materials, by weight, 200 parts of dimethyl silicone oil (average kinematic viscosity 500, 1000 compounded in a weight ratio of 2: 3), 20 parts of polytetrafluoroethylene powder (average fineness 40nm, 80nm, 120nm compounded in a weight ratio of 1: 2: 3), 0.5 part of a polyazole modified carbon nanotube, 20 parts of sodium hydroxide, 8 parts of boron nitride, 2.5 parts of diphenylamine and 2.5 parts of hydroquinone.
The dimethylsilicone oil used in this comparative example was the same as in example 1.
The polyacene modified carbon nanotubes used in this comparative example were the same as in example 1.
The multi-walled carbon nanotubes used in this comparative example were the same as in example 1.
The metallocene used in this comparative example was the same as in example 1.
The comparative example also provides a method for preparing the long-acting high-temperature lubricating grease: (1) weighing dimethyl silicone oil, polytetrafluoroethylene powder, a polybenzazole modified carbon nano tube and boron nitride, heating to 120 ℃, stirring and reacting for 3 hours; (2) adding sodium hydroxide into the step (1), and then performing saponification reaction at 130 ℃ for 6 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 200 ℃ for high-temperature refining, wherein the reaction time is 4 hours, cooling to 100 ℃, finally adding diphenylamine and hydroquinone, and homogenizing, degassing and filtering to obtain the long-acting high-temperature lubricating grease. This grease was designated as D3.
Comparative example 4
Comparative example 4 provides a long-acting high-temperature lubricating grease, and the raw materials comprise, by weight, 200 parts of dimethicone (average kinematic viscosity 500, 1000 compounded in a weight ratio of 2: 3), 20 parts of polytetrafluoroethylene powder (average fineness 40nm, 80nm, 120nm compounded in a weight ratio of 1: 2: 3), 8 parts of polyazole modified carbon nanotube, 20 parts of sodium hydroxide, 8 parts of boron nitride, 2.5 parts of diphenylamine, and 2.5 parts of hydroquinone.
The dimethylsilicone oil used in this comparative example was the same as in example 1.
The polyacene modified carbon nanotubes used in this comparative example were the same as in example 1.
The multi-walled carbon nanotubes used in this comparative example were the same as in example 1.
The metallocene used in this comparative example was the same as in example 1.
The comparative example also provides a method for preparing the long-acting high-temperature lubricating grease: (1) weighing dimethyl silicone oil, polytetrafluoroethylene powder, a polybenzazole modified carbon nano tube and boron nitride, heating to 120 ℃, stirring and reacting for 3 hours; (2) adding sodium hydroxide into the step (1), and then performing saponification reaction at 130 ℃ for 6 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 200 ℃ for high-temperature refining, wherein the reaction time is 4 hours, cooling to 100 ℃, finally adding diphenylamine and hydroquinone, and homogenizing, degassing and filtering to obtain the long-acting high-temperature lubricating grease. This grease was designated as D4.
Comparative example 5
Comparative example 5 provides a long-acting high-temperature lubricating grease, which comprises the following raw materials, by weight, 200 parts of dimethyl silicone oil (average kinematic viscosity 500, 1000 compounded in a weight ratio of 2: 3), 20 parts of polytetrafluoroethylene powder (average fineness 40nm, 80nm, 120nm compounded in a weight ratio of 1: 1: 5), 5 parts of a polyazole modified carbon nanotube, 20 parts of sodium hydroxide, 8 parts of boron nitride, 2.5 parts of diphenylamine and 2.5 parts of hydroquinone.
The dimethylsilicone oil used in this comparative example was the same as in example 1.
The polyacene modified carbon nanotubes used in this comparative example were the same as in example 1.
The multi-walled carbon nanotubes used in this comparative example were the same as in example 1.
The metallocene used in this comparative example was the same as in example 1.
The comparative example also provides a method for preparing the long-acting high-temperature lubricating grease: (1) weighing dimethyl silicone oil, polytetrafluoroethylene powder, a polybenzazole modified carbon nano tube and boron nitride, heating to 120 ℃, stirring and reacting for 3 hours; (2) adding sodium hydroxide into the step (1), and then performing saponification reaction at 130 ℃ for 6 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 200 ℃ for high-temperature refining, wherein the reaction time is 4 hours, cooling to 100 ℃, finally adding diphenylamine and hydroquinone, and homogenizing, degassing and filtering to obtain the long-acting high-temperature lubricating grease. This grease was designated as D5.
Comparative example 6
Comparative example 6 provides a long-acting high-temperature lubricating grease, which comprises the following raw materials, by weight, 200 parts of simethicone (with an average kinematic viscosity of 500, compounded at a weight ratio of 2: 3 to 1000), 20 parts of polytetrafluoroethylene powder (compounded at an average fineness of 40nm, 80nm and 120nm at a weight ratio of 1: 2: 3), 5 parts of a polyazole modified carbon nanotube, 20 parts of sodium hydroxide, 8 parts of boron nitride, 5 parts of diphenylamine and 2.5 parts of hydroquinone.
The dimethylsilicone oil used in this comparative example was the same as in example 1.
The polyacene modified carbon nanotubes used in this comparative example were the same as in example 1.
The multi-walled carbon nanotubes used in this comparative example were the same as in example 1.
The metallocene used in this comparative example was the same as in example 1.
The comparative example also provides a method for preparing the long-acting high-temperature lubricating grease: (1) weighing dimethyl silicone oil, polytetrafluoroethylene powder, a polybenzazole modified carbon nano tube and boron nitride, heating to 120 ℃, stirring and reacting for 3 hours; (2) adding sodium hydroxide into the step (1), and then performing saponification reaction at 130 ℃ for 6 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 200 ℃ for high-temperature refining, wherein the reaction time is 4 hours, cooling to 100 ℃, finally adding diphenylamine and hydroquinone, and homogenizing, degassing and filtering to obtain the long-acting high-temperature lubricating grease. This grease was designated as D6.
Comparative example 7
Comparative example 7 provides a long-acting high-temperature lubricating grease, which comprises the following raw materials, by weight, 200 parts of dimethyl silicone oil (average kinematic viscosity 500, 1000 compounded in a weight ratio of 2: 3), 20 parts of polytetrafluoroethylene powder (average fineness 40nm, 80nm, 120nm compounded in a weight ratio of 1: 2: 3), 5 parts of a polyazacene modified carbon nanotube, 20 parts of sodium hydroxide, 8 parts of boron nitride and 2.5 parts of diphenylamine.
The dimethylsilicone oil used in this comparative example was the same as in example 1.
The polyacene modified carbon nanotubes used in this comparative example were the same as in example 1.
The multi-walled carbon nanotubes used in this comparative example were the same as in example 1.
The metallocene used in this comparative example was the same as in example 1.
The comparative example also provides a method for preparing the long-acting high-temperature lubricating grease: (1) weighing dimethyl silicone oil, polytetrafluoroethylene powder, a polynitrogen cyclopentadiene modified carbon nano tube and boron nitride, heating to 120 ℃, stirring, and reacting for 3 hours; (2) adding sodium hydroxide into the step (1), and then performing saponification reaction at 130 ℃ for 6 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary finished product obtained in the step (2) to 200 ℃ for high-temperature refining, wherein the reaction time is 4 hours, cooling to 100 ℃, finally adding diphenylamine, and homogenizing, degassing and filtering to obtain the long-acting high-temperature lubricating grease. This grease was designated as D7.
Comparative example 8
Comparative example 8 provides a long-acting high-temperature lubricating grease, which comprises the following raw materials, by weight, 200 parts of simethicone (with an average kinematic viscosity of 500, compounded at a weight ratio of 2: 3 to 1000), 20 parts of polytetrafluoroethylene powder (compounded at an average fineness of 40nm, 80nm, and 120nm at a weight ratio of 1: 2: 3), 5 parts of a polyazole modified carbon nanotube, 20 parts of sodium hydroxide, 8 parts of boron nitride, and 2.5 parts of hydroquinone.
The dimethylsilicone oil used in this comparative example was the same as in example 1.
The polyacene modified carbon nanotubes used in this comparative example were the same as in example 1.
The multi-walled carbon nanotubes used in this comparative example were the same as in example 1.
The metallocene used in this comparative example was the same as in example 1.
The comparative example also provides a method for preparing the long-acting high-temperature lubricating grease: (1) weighing dimethyl silicone oil, polytetrafluoroethylene powder, a polybenzazole modified carbon nano tube and boron nitride, heating to 120 ℃, stirring and reacting for 3 hours; (2) adding sodium hydroxide into the step (1), and then performing saponification reaction at 130 ℃ for 6 hours to obtain a lubricating grease primary finished product; (3) and (3) heating the primary product obtained in the step (2) to 200 ℃ for high-temperature refining, wherein the reaction time is 4 hours, cooling to 100 ℃, finally adding hydroquinone, and homogenizing, degassing and filtering to obtain the long-acting high-temperature lubricating grease. This grease was designated as D8.
Evaluation of Performance
1. And (3) drop point testing: the dropping point is the lowest temperature at which the grease begins to drop when melted by heat, and is one of the important indicators of the grease. Is an index of the temperature resistance of the lubricating grease. Test methods 5 samples were tested per example according to the national standard GB/T4929-85, and the dropping points measured were averaged and reported in Table 1.
2. High-temperature evaporation loss: the high-temperature evaporation loss refers to the loss proportion of the lubricating grease at a high temperature within a certain time, the evaporation loss is in direct proportion to the volatility of an oil product, and the greater the evaporation loss is, the greater the oil consumption in actual use is. The test method is national standard GB/T7325 (200 ℃, 22h), 5 samples are tested in each example, and the loss ratios measured are averaged and reported in Table 1.
3. Working cone penetration: cone penetration is an index that measures the consistency and hardness of grease and is the depth at which a cone falls into a sample under specified load, time and temperature conditions. The unit is expressed in 0.1 mm. A higher penetration value indicates a softer grease and conversely a harder grease. Method for testing penetration the apparatus was a penetration tester, the method was national standard GB/T269-91, 5 specimens were tested for each example, the measured loss ratios were averaged and reported in table 1.
TABLE 1
Lubricating grease Dropping Point (. degree.C.) Loss of evaporation (%) Penetration degree (0.1mm)
R1 391 0.11 349
R2 387 0.28 331
R3 388 0.17 341
R4 377 0.21 325
R5 379 0.19 339
R6 381 0.25 331
R7 386 0.26 324
R8 390 0.19 337
D1 277 1.54 266
D2 156 3.21 211
D3 321 0.91 280
D4 344 1.16 293
D5 295 2.56 233
D6 313 1.26 276
D7 299 2.85 311
D8 287 3.01 289
The long-acting high-temperature lubricating grease provided by the invention has excellent temperature resistance, curing degree, softness and use aging, is suitable for popularization and use in the field of high-temperature lubricating grease, and has a wide development prospect as can be known from examples 1-8 and comparative examples 1-8. Wherein example 1 achieves the best dropping point, the least evaporation loss and the highest softness and high temperature stability with the best raw material weight ratio, fineness and the like.
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. A long-acting high-temperature lubricating grease is characterized in that: the raw materials comprise, by weight, 70-200 parts of base oil, 10-20 parts of a thickening agent, 1-5 parts of modified carbon nanotubes, 5-20 parts of a saponification reaction agent, 1-8 parts of an additive and 1-5 parts of an auxiliary additive.
2. The long-acting high temperature grease of claim 1, wherein: the base oil is at least one of dimethyl silicone oil, ethyl silicone oil, phenyl silicone oil, methyl hydrogen-containing silicone oil, methyl phenyl silicone oil, methyl chlorphenyl silicone oil and naphthenic base rubber silicone oil; the thickening agent is at least one of polytetrafluoroethylene, composite calcium sulfonate, composite lithium, composite aluminum, bentonite, polyurea and polyethylene; the saponification reactant is at least one of sodium hydroxide, potassium hydroxide, calcium hydroxide, lithium hydroxide and concentrated ammonia water; the additive is at least one of boron nitride, graphite, metal powder, stearic acid and boric acid; the auxiliary additive is at least one of diphenylamine, ethylene diamine tetraacetic acid tetrabenzyl amide, hydroquinone, thiobisphenol and triphenol.
3. The long-acting high temperature grease of claim 2, wherein: the base oil is dimethyl silicone oil with average viscosity of 400-600, and the base oil is dimethyl silicone oil with average viscosity of 700-1000.
4. The long-acting high temperature grease of claim 3, wherein: the weight ratio of the simethicone with the average viscosity of 400-600 to the simethicone with the average viscosity of 700-1000 is (1-3): (2-4).
5. The long-acting high temperature grease of claim 1, wherein: the modified carbon nano tube is a polyazole modified carbon nano tube.
6. The long-acting high temperature grease of claim 5, wherein: the weight ratio of the polyacene modified carbon nano tube to the base oil is 1: (40-200).
7. The long-acting high temperature grease of claim 6, wherein: the thickening agent is PTFE with the average fineness of 40nm, PTFE with the average fineness of 80nm and PTFE with the average fineness of 120 nm.
8. The long-acting high temperature grease of claim 7, wherein: PTFE with the average fineness of 40nm, wherein the weight ratio of the PTFE with the average fineness of 80nm to the PTFE with the average fineness of 120nm is (1-3): (1-3): (1-3).
9. The long-acting high temperature grease of claim 8, wherein: the auxiliary additive is diphenylamine and hydroquinone.
10. The preparation method of the long-acting high-temperature lubricating grease as claimed in any one of claims 1 to 9, characterized by comprising the following steps: (1) weighing the base oil, the thickening agent, the modified carbon nano tube and the 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 long-acting high-temperature lubricating grease.
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Citations (5)

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