CN113046149B - Lubricating grease containing composite additive and preparation method thereof - Google Patents
Lubricating grease containing composite additive and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- 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
- C10M169/04—Mixtures of base-materials and additives
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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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
- C10M2207/1285—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof used as thickening agents
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/40—Fatty vegetable or animal oils
- C10M2207/401—Fatty vegetable or animal oils used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/22—Heterocyclic nitrogen compounds
- C10M2215/223—Five-membered rings containing nitrogen and carbon only
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- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention discloses lubricating grease containing a composite additive and a preparation method thereof, wherein the composite additive in the lubricating grease comprises nano graphene and benzotriazole derivatives, and the mass percent of the graphene prepared by an electrolytic method in the lubricating grease is 0.01-1.0%; the mass percentage of the benzotriazole derivative in the lubricating grease is 0.5-5.0%; adding nano graphene and benzotriazole derivatives before saponification. The invention has obvious beneficial effects: (1) the benzotriazole derivatives can fully disperse the additive and increase the mixing degree of the nano material; (2) the low-price pure rapeseed oil is utilized, and the lubricating grease is environment-friendly; (3) the unmodified nano graphene has wide application range, and the lubricating grease containing the nano graphene has good tribological performance and thermal stability.
Description
Technical Field
The invention relates to the technical field of lubrication, in particular to lubricating grease containing a compound additive and a preparation method thereof.
Background
Nanotechnology is a new emerging technology in new century and is applied to a plurality of fields such as environment, materials, communication, processing and the like. The nano material is more concerned by various countries, and under the promotion of the sustainable development concept of economy in China, the related research of the nano material creates a new chapter. Through the cross-technological research of various disciplines, the modification work of how to apply nano materials and develop novel nano materials is in the spotlight. As the rare earth resources in China are rich, a plurality of scientific researchers introduce nanotechnology into the field of rare earth industry.
The addition of nano-graphene to lubricating oil has been studied. The Wangxingbo et al disclose a graphene oxide modification-based nano additive and application thereof, wherein graphene oxide is modified by utilizing polymer phosphate, and the nano additive can form a stable dispersion system in polyether and has good thermal stability.
Lin and the like utilize stearic acid as a modifier, stearic acid grafted graphene is prepared by a chemical modification method, hydrophilic groups on the surface of the graphene are reduced due to the existence of long-chain alkane on the surface of the graphene, the compatibility of the graphene and base oil is enhanced, and the prepared lubricating oil has lower and more stable friction coefficient and higher bearing abrasion resistance.
The addition of nanomaterial additives to greases has also been investigated. Chinese patent CN101205495A discloses a composite nano particle, lubricating grease containing the composite nano particle and a preparation method thereof, and invents a compound of dithiodiazolethione and butoxy-triethylene glycol and LaF 3 After the composite nano-particles are added with lubricating grease, the friction effect is obvious. Chinese patent CN102911774A discloses a lubricating grease containing carbon nanotubes and a preparation method thereof, bentonite is used as a thickening agent, base oil is refined mineral oil and synthetic oil, and the lubricating grease containing carbon nanotubes is added, so that the wear resistance is improved. For other nano material additives, Chinese patent CN102492523A introduces a mixed nano lubricating grease additive and its application, and describes other types of inorganic nano additives, Cu, Al and Al 2 O 3 The nano composite additive composed of metal powder shows that inorganic powder can also be added into the lubricating grease to achieve good friction effect. Study on tribological properties of benzotriazole-modified nanoparticles 2 And nano La 2 O 3 Tribological properties in diesel engines and lithium-based greases were investigated. However, the modified nanometer rare earth oxide has unstable structure and is easy to precipitate(ii) a The modification is needed only under a certain specific working condition or special requirement, and the application range is limited. In addition, the addition of additives after saponification of the grease causes problems such as uneven dispersion of the additives, small degree of mixing between soap particles, and insignificant lubricating effect.
The ethyl benzotriazole acetate and butyl benzotriazole acetate have certain oil solubility and can be used as lubricating oil additives. Benzotriazole is solid, has poor oil solubility, cannot be used in lubricating oil, and is mainly used as an additive of paint, plastics, medicines, pesticides and dyes. Therefore, aiming at the defects of the current lubricating grease, the research and development of novel high-performance lubricating grease is the current main direction of research.
Disclosure of Invention
The invention aims to provide lubricating grease containing a composite additive and a preparation method thereof, which are used for solving the problems in the prior art, environment-friendly vegetable oil is utilized to saponify to form calcium-based grease or lithium-calcium-based grease, and nano graphene and benzotriazole derivatives are added before saponification.
In order to achieve the purpose, the invention provides the following scheme: the invention provides lubricating grease containing a composite additive, wherein the lubricating grease contains the composite additive, the composite additive comprises nano-graphene and benzotriazole derivatives, the content of the nano-graphene in the lubricating grease is 0.01-1.0 wt%, and the content of the benzotriazole derivatives in the lubricating grease is 0.5-5.0 wt%.
As a further optimization of the present invention, the grease is a calcium-based grease or a calcium-lithium-based grease.
As further optimization of the invention, the content of the nano graphene in the lubricating grease is 0.01-0.5 wt%, and the content of the benzotriazole derivative in the lubricating grease is 0.5-3.0 wt%.
As further optimization of the invention, the nano graphene is prepared by an electrolytic method, the granularity of the nano graphene is 0.5-50 nm, and the benzotriazole derivative is benzotriazole acetate.
As a further optimization of the invention, the benzotriazole acetate comprises one of benzotriazole ethyl acetate, benzotriazole butyl acetate and benzotriazole n-octyl acetate.
The invention provides a preparation method of the lubricating grease containing the composite additive, which is characterized in that the nano graphene and the benzotriazole derivative are added before saponification.
As a further optimization of the invention, the preparation method comprises the following steps,
(1) sequentially weighing base oil, a thickening agent, nano-graphene and benzotriazole derivatives according to the mass ratio of (5-10) to 1 to (0.004-0.01) to (0.15-0.25), uniformly mixing the thickening agent and 30-50% of the base oil, adding the nano-graphene and the benzotriazole derivatives, and stirring and mixing for 10-20min to obtain a first mixed solution;
(2) putting the first mixed solution obtained in the step (1) into a reaction vessel, and introducing N 2 Adding an inorganic alkali solution to obtain a second mixed solution, heating the second mixed solution for saponification, adding 30% base oil when the second mixed solution is changed from a liquid state to a semi-fluid state or a solid state, and then continuously saponifying for 1-1.5h, wherein the optimal time is 1 h;
(3) heating the second mixed solution of which the state is not changed after the reaction in the step (2) is finished to remove water until no water drops or water vapor is generated to obtain a third mixed solution;
(4) and (4) adding the residual base oil into the third mixed solution obtained in the step (3) to obtain a fourth mixed solution, heating the fourth mixed solution for refining at high temperature until the fourth mixed solution is changed from a dilute solid state to a true solution state, keeping the temperature for 5-15min, cooling to 120 ℃, stirring for 0.5h, cooling to room temperature, and collecting lubricating grease.
As a further optimization of the invention, the mass ratio of the base oil to the thickening agent in the step (1) is (5-7):1, the base oil is pure rapeseed oil without any treatment, and the thickening agent is 12-hydroxystearic acid.
As a further optimization of the invention, the mass ratio of the inorganic alkali solution to the thickening agent in the step (2) is 112: 10-15, and the inorganic alkali solution is 10 wt% of inorganic alkali water solution; the inorganic base comprises at least one of calcium hydroxide and lithium hydroxide, and the saponification temperature is 115-125 ℃, and the optimal saponification temperature is 120 ℃.
As a further optimization of the invention, the mass ratio of the calcium hydroxide to the lithium hydroxide is 1: 2.
As a further optimization of the invention, the water removal in the step (3) is 145-155 ℃ for 1-1.5h, and the optimal water removal is 150 ℃; the high-temperature refining temperature in the step (4) is 215-225 ℃, and the optimal temperature is 220 ℃.
The invention discloses the following technical effects:
(1) according to the invention, the benzotriazole derivatives are added before saponification and fatting, so that the additive nano graphene can be fully dispersed, and the mixing degree of the nano material is increased; when the soap particles are formed, the nano materials are favorably attached or dispersed;
(2) the invention utilizes the environment-friendly base oil, namely the rapeseed oil, which is environment-friendly lubricating grease;
(3) the invention makes full use of the excellent tribological performance of the benzotriazole nitrogen-containing heterocycle.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a flow chart of the preparation process of the grease containing the complex additive according to the present invention.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
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. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated herein by reference to disclose and describe the methods and/or materials in connection with which the documents are cited. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including but not limited to.
Example 1
60g of rapeseed oil, 12.0g of 12-hydroxystearic acid, 0.07g of nano graphene and 1.8g of ethyl benzotriazole acetate are prepared.
24.0g of rapeseed oil, 12.0g of 12-hydroxystearic acid, 0.07g of nano graphene and 1.8g of ethyl benzotriazole acetate are stirred and mixed for 20min in advance, transferred into a reaction container, and slowly dripped with 112.0g of prepared 10 wt% calcium hydroxide solution after nitrogen is introduced. Then the temperature is increased to 120 ℃ for saponification reaction, the saponification reaction is carried out for 1h, the reactant is changed from liquid state to semi-fluid state or solid state, then 18.0g of rapeseed oil is added, and the saponification is continued for 1.5 h. And after the state of the reactant is not changed, heating to 150 ℃ to remove water for 1 h. When no water drop and no water vapor exist, 18.0g of rapeseed oil is added, the temperature is raised to 218 ℃, and when the reactant reaches a true solution state from a dilute solid state, the reaction is kept for 10 min. And after naturally cooling to 120 ℃, continuously stirring for 0.5h, naturally cooling again, and collecting lubricating grease.
The nano graphene in the embodiment is prepared by an electrolytic method and has a particle size of 20 nm.
Example 2
100.0g of rapeseed oil, 15.0g of 12-hydroxystearic acid, 0.07g of nano graphene and 2.0g of ethyl benzotriazole acetate are prepared.
40.0g of rapeseed oil, 15.0g of 12-hydroxystearic acid, 0.07g of nano-graphene and 2.0g of ethyl benzotriazole acetate are stirred and mixed for 20min in advance, the mixture is moved into a reaction vessel and nitrogen is introduced, and then 112.0g of prepared 10 wt% calcium hydroxide solution is slowly dripped. Then the temperature is increased to 120 ℃ for saponification reaction, the saponification reaction is carried out for 1h, the reactant is changed from liquid state to semi-fluid state or solid state, then 30.0g of rapeseed oil is added, and the saponification is continued for 1.5 h. After the state of the reactant is not changed, the temperature is raised to 150 ℃ to remove water for 1 h. When no water drop and no water vapor exist, 30.0g of rapeseed oil is added, the temperature is raised to 218 ℃, and when the reactant reaches a true solution state from a dilute solid state, the reaction is kept for 10 min. And after naturally cooling to 120 ℃, stirring for 0.5h, naturally cooling again, and collecting lubricating grease.
The nano graphene in the embodiment is prepared by an electrolytic method and has a particle size of 50 nm.
Example 3
60.0g of rapeseed oil, 12.0g of 12-hydroxystearic acid, 0.05g of nano graphene and 2.0g of benzotriazole butyl acetate are prepared.
24.0g of rapeseed oil, 12.0g of 12-hydroxystearic acid, 0.05g of nano graphene and 2.0g of benzotriazole butyl acetate are stirred and mixed for 20min in advance, transferred into a reaction container, and slowly dripped with 112.0g of prepared 10 wt% calcium hydroxide solution after nitrogen is introduced. Then the temperature is increased to 120 ℃ for saponification reaction, the saponification reaction is carried out for 1h, the reactant is changed from liquid state to semi-fluid state or solid state, then 18.0g of rapeseed oil is added, and the saponification is continued for 1.5 h. And after the state of the reactant is not changed, heating to 150 ℃ to remove water for 1 h. When no water drops and no water vapor exist, 18.0g of rapeseed oil is added, the temperature is raised to 218 ℃, and when the reactant reaches a true solution state from a dilute solid state, the reactant is kept for 10 min. After naturally cooling to 120 ℃, continuously stirring for 0.5h, naturally cooling again, and collecting lubricating grease.
The nano graphene in the embodiment is prepared by an electrolytic method and has the granularity of 1 nm.
Example 4
60.0g of rapeseed oil, 12.0g of 12-hydroxystearic acid, 0.08g of nano graphene and 1.8g of benzotriazole butyl acetate are prepared.
30.0g of rapeseed oil, 12.0g of 12-hydroxystearic acid, 0.08g of nano graphene and 1.8g of benzotriazole butyl acetate are stirred and mixed for 20min in advance, transferred into a reaction container, and slowly dripped with 112.0g of prepared 10 wt% calcium hydroxide solution after nitrogen is introduced. Then the temperature is raised to 120 ℃ for saponification reaction, the reactant is changed from liquid state to semi-fluid or solid state after saponification reaction for 1h, 18.0g of rapeseed oil is added, and saponification is continued for 1.5 h. After the state of the reactant is not changed, the temperature is raised to 150 ℃ to remove water for 1 h. When no water drop and no water vapor exist, 12.0g of rapeseed oil is added, the temperature is raised to 218 ℃, and when the reactant reaches a true solution state from a dilute solid state, the reaction is kept for 10 min. After naturally cooling to 120 ℃, continuously stirring for 0.5h, naturally cooling again, and collecting lubricating grease.
The nano graphene in the embodiment is prepared by an electrolytic method and has the particle size of 15 nm.
Example 5
54.0g of rapeseed oil, 10.0g of 12-hydroxystearic acid, 0.07g of nano graphene and 2.5g of benzotriazole acetic acid n-octyl ester are prepared.
24.0g of rapeseed oil, 10.0g of 12-hydroxystearic acid, 0.07g of nano graphene and 2.5g of benzotriazole acetic acid n-octyl ester are stirred and mixed for 20min in advance, the mixture is moved into a reaction container, nitrogen is introduced, and then 112.0g of prepared 10 wt% calcium hydroxide and lithium hydroxide solution are slowly dripped, wherein the mass ratio of the calcium hydroxide to the lithium hydroxide is 1: 2. Then the temperature is increased to 120 ℃ for saponification reaction, the saponification reaction is carried out for 1h, the reactant is changed from liquid state to semi-fluid state or solid state, then 16.2g rapeseed oil is added, and the saponification is continued for 1.5 h. After the state of the reactant is not changed, the temperature is raised to 150 ℃ to remove water for 1 h. When no water drop and no water vapor exist, 13.8g of rapeseed oil are added, the temperature is raised to 218 ℃, and when the reactant reaches a true solution state from a dilute solid state, the reaction is kept for 10 min. And after naturally cooling to 120 ℃, continuously stirring for 0.5h, naturally cooling again, and collecting lubricating grease.
The nano graphene in the embodiment is prepared by an electrolytic method and has the granularity of 20 nm.
Example 6
100.0g of rapeseed oil, 15.0g of 12-hydroxystearic acid, 0.17g of nano-sized caryophyllene and 2.8g of benzotriazole acetic acid n-octyl ester are prepared.
40.0g of rapeseed oil, 15.0g of 12-hydroxystearic acid, 0.17g of nano graphene and 2.8g of n-octyl benzotriazole acetate are stirred and mixed for 20min in advance, the mixture is moved into a reaction container, nitrogen is introduced, and then 112.0g of prepared 10 wt% calcium hydroxide and lithium hydroxide solution are slowly dripped, wherein the mass ratio of the calcium hydroxide to the lithium hydroxide is 1: 2. Then the temperature is increased to 120 ℃ for saponification reaction, the saponification reaction is carried out for 1h, the reactant is changed from liquid state to semi-fluid state or solid state, then 30.0g of rapeseed oil is added, and the saponification is continued for 1.5 h. And after the state of the reactant is not changed, heating to 150 ℃ to remove water for 1 h. When no water drop exists, 30.0g of rapeseed oil is added, the temperature is raised to 220 ℃, and when the reactant reaches a true solution state from a dilute solid state, the reaction is kept for 10 min. After naturally cooling to 120 ℃, continuously stirring for 0.5h, naturally cooling again, and collecting lubricating grease.
The nano graphene in the embodiment is prepared by an electrolytic method and has the granularity of 30 nm.
Comparative example 1
The method is the same as that in example 1, except that nano graphene and benzotriazole derivatives are not added, and rapeseed oil is selected as the base oil.
Experimental example 1
Performance test analysis
1. Extreme pressure bearing capacity performance test analysis
The greases prepared in examples 1-6 and the grease prepared in comparative example 1 were tested for extreme pressure bearing capacity and the data obtained are shown in table 1.
TABLE 1 extreme pressure bearing Capacity of greases containing Complex additives
| Examples | Comparative example 1 | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| Extreme pressure value/N | 513 | 962 | 753 | 826 | 998 | 953 | 1038 |
From table 1, it can be seen that when the mass fraction of the nano graphene contained in the grease using rapeseed oil as the base oil is 0.05% to 0.5%, and the mass fraction of the benzotriazole derivative is in the range of 2.0% to 3.5%, the extreme pressure values of the greases are greater than those of the greases containing no additive, which indicates that the extreme pressure bearing capacity is significantly improved when the compound additive is added to the grease.
2. Analysis of abrasion resistance test
Grease prepared in comparative example 1 and examples 1 to 6 was subjected to a long-grinding experiment using a vertical universal friction wear tester, model MMW-1, manufactured by shun yao tester ltd, for 30min, at a load of 392N and at a rotation speed of 1450 r/min. The wear-leveling diameter (WSD) of the test ball was measured using a reading microscope (precision. + -. 0.01) according to SH/T0189-92(392N) standard, and the average of the three wear-leveling diameters was taken as the experimental result value. The selected steel ball is a second grade G16 standard steel ball (national standard GB/T308-2002) produced by Guangming Steel ball factory in Xiui county, the diameter is 12.7mm, the hardness HRC is 59-61, and the weight is 2.5 Kg.
Table 2 lists the grease wear point data prepared for comparative example 1 and examples 1-6. As shown in Table 2, the antiwear properties of the greases containing the complex additives were better than those of the pure greases.
TABLE 2392N Wear Scar Diameter (WSD) for greases
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (8)
1. The lubricating grease containing the composite additive is characterized in that the lubricating grease contains the composite additive, the composite additive comprises nano graphene and benzotriazole derivatives, the nano graphene accounts for 0.01-1.0 wt% of the lubricating grease, and the benzotriazole derivatives account for 0.5-5.0 wt% of the lubricating grease;
the nano graphene is nano graphene with the granularity of 0.5nm-50nm, and the benzotriazole derivative is benzotriazole acetate;
the preparation method of the lubricating grease containing the composite additive comprises the following steps: and adding the nano graphene and the benzotriazole derivative before saponification.
2. The grease containing the complex additive as claimed in claim 1, wherein the grease is a calcium-based grease or a calcium-lithium-based grease.
3. The grease containing the complex additive as claimed in claim 1, wherein the content of the nano graphene in the grease is 0.01 wt% -0.5 wt%, and the content of the benzotriazole derivative in the grease is 0.5 wt% -3.0 wt%.
4. The lubricating grease containing the composite additive according to claim 1, wherein the benzotriazole acetate comprises one of benzotriazole ethyl acetate, benzotriazole butyl acetate, and benzotriazole n-octyl acetate.
5. The grease containing complex additive as claimed in claim 1, wherein the preparation method comprises the steps of,
(1) sequentially weighing base oil, a thickening agent, nano-graphene and benzotriazole derivatives according to the mass ratio of (5-10) to 1 to (0.004-0.01) to (0.15-0.25), uniformly mixing the thickening agent and 30-50% of the base oil, adding the nano-graphene and the benzotriazole derivatives, and stirring and mixing for 10-20min to obtain a first mixed solution;
(2) putting the first mixed solution obtained in the step (1) into a reaction vessel, and introducing N 2 Adding an inorganic alkali solution to obtain a second mixed solution, heating the second mixed solution for saponification, adding 30% of base oil when the second mixed solution is changed from a liquid state to a semi-fluid state or a solid state, and then continuing saponification for 1-1.5 hours;
(3) heating the saponified second mixed solution obtained in the step (2) to remove water to obtain a third mixed solution;
(4) and (4) adding the residual base oil into the third mixed solution obtained in the step (3) to obtain a fourth mixed solution, heating the fourth mixed solution for refining until the fourth mixed solution is changed into a true solution state from a dilute solid state, keeping for 5-15min, cooling to 120 ℃, stirring for 0.5h, cooling to room temperature, and collecting lubricating grease.
6. The grease containing the complex additive as claimed in claim 5, wherein the mass ratio of the base oil to the thickener in step (1) is (5-7):1, the base oil is rapeseed oil, and the thickener is 12-hydroxystearic acid.
7. The grease containing complex additive as claimed in claim 5, wherein the mass ratio of the inorganic base solution to the thickener in step (2) is 112: 10-15, and the inorganic base solution is 10 wt% inorganic base solution; the inorganic alkali comprises at least one of calcium hydroxide and lithium hydroxide, and the saponification temperature is 115-125 ℃.
8. The grease containing complex additive as claimed in claim 5, wherein the water removal in step (3) is 145-155 ℃ for 1-1.5 h; the high-temperature refining temperature in the step (4) is 215-225 ℃.
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| CN104560289B (en) * | 2013-10-28 | 2017-11-03 | 中国石油化工股份有限公司 | A kind of lithium base grease and preparation method thereof |
| CN109439398B (en) * | 2018-11-30 | 2021-06-29 | 新疆金雪驰科技股份有限公司 | Lubricating grease containing composite additive and preparation method thereof |
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