CN113150858B - Composite barium-based lubricating grease and preparation method thereof - Google Patents

Composite barium-based lubricating grease and preparation method thereof Download PDF

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CN113150858B
CN113150858B CN202110311340.6A CN202110311340A CN113150858B CN 113150858 B CN113150858 B CN 113150858B CN 202110311340 A CN202110311340 A CN 202110311340A CN 113150858 B CN113150858 B CN 113150858B
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barium
preparing
composite
grease
temperature
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CN113150858A (en
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樊星
颜扬扬
莫文龙
姚婷
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Suzhou Aigu New Material Co ltd
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Suzhou Aigu New Material Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/22—Compounds containing sulfur, selenium or tellurium
    • 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
    • C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
    • 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
    • C10M2201/04—Elements
    • C10M2201/05—Metals; Alloys
    • 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
    • C10M2201/065—Sulfides; Selenides; Tellurides
    • 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
    • C10M2201/065—Sulfides; Selenides; Tellurides
    • C10M2201/066—Molybdenum sulfide
    • 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
    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/123—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
    • C10M2207/1236—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic used as thickening agent
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/124—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms containing hydroxy groups; Ethers thereof
    • C10M2207/1245—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms containing hydroxy groups; Ethers thereof used as thickening agent
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
    • C10M2207/1265—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic used as thickening agent
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/127—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids polycarboxylic
    • C10M2207/1276—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids polycarboxylic used as thickening agent
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
    • C10M2207/1285—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof used as thickening agents
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/287—Partial esters
    • C10M2207/289—Partial esters containing free hydroxy groups
    • C10M2207/2895—Partial esters containing free hydroxy groups used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/32—Esters of carbonic acid
    • C10M2207/325—Esters of carbonic acid used as base material

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  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

The application relates to a composite barium-based lubricating grease and a preparation method thereof, wherein the preparation method comprises the following steps: mixing and heating fatty acid and base oil with the mass A, and adding the base oil with the mass B and barium hydroxide octahydrate for saponification reaction when the temperature of the mixed solution is increased to 100-110 ℃; gradually heating the reaction solution after the saponification reaction to 120-130 ℃, exhausting steam, adding small molecular organic acid and tungsten disulfide powder or modified tungsten disulfide powder, and stirring at constant temperature; heating the mixed solution to 170-200 ℃, and refining at high temperature; reducing the temperature of the mixed solution after high-temperature refining to be below 170 ℃, quickly heating the mixed solution to 170-200 ℃, and keeping the temperature for a period of time; and (3) when the temperature of the mixed solution is reduced to be below 80 ℃, homogenizing and degassing the mixed solution to obtain the composite barium-based lubricating grease. The composite barium-based lubricating grease has the advantages of excellent wear resistance, high temperature resistance, long service life and the like.

Description

Composite barium-based lubricating grease and preparation method thereof
Technical Field
The application belongs to the technical field of lubricant preparation, and particularly relates to a composite barium-based lubricating grease and a preparation method thereof.
Background
The composite barium-based lubricating grease is prepared from medium-viscosity mineral oil thickened and refined by composite barium soap generated by the reaction of two or more acids and barium hydroxide, has good water resistance, higher dropping point and certain protective performance, has very strong water resistance and pressure resistance of composite barium-based lubricating grease-ZB 10-2 prepared from barium stearate thickened low-condensation-point synthetic transformer oil fraction, has good adhesion and protective performance to metal surfaces, is almost insoluble in organic solvents such as gasoline, alcohol and the like, and can be used for lubricating parts in contact with acid, alkali or organic solvents in the chemical industry.
In recent years, with the development of modern industry, increasingly strict requirements on the quality of lubricating grease are provided for industrial departments such as bearings, automobiles, printing and dyeing, mines, metallurgy, aerospace and the like, and a plurality of lubricating parts are filled with grease once and are not supplemented or replaced in the operation process, so that the requirements on the service life, high temperature resistance and wear resistance of the lubricating grease are high, and the use of the composite barium-based lubricating grease is limited.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at solving the defects in the prior art, the composite barium-based lubricating grease and the preparation method thereof are provided, and the purpose is to enable the composite barium-based lubricating grease to have long service life, strong extreme pressure abrasion resistance and high temperature resistance.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of composite barium-based lubricating grease comprises the following steps:
s1: mixing and heating fatty acid and base oil with the mass A, adding the base oil with the mass B and barium hydroxide octahydrate when the temperature of the mixed solution is increased to 100-110 ℃, and performing saponification reaction, wherein the ratio of the mass A to the mass B is 1: 1.5-2.5;
s2: gradually heating the reaction solution after the saponification reaction to 120-130 ℃, exhausting steam, adding small molecular organic acid and tungsten disulfide powder or modified tungsten disulfide powder, and stirring at constant temperature;
s3: heating the mixed solution obtained in the step S2 to 170-200 ℃, and refining at a high temperature;
s4: reducing the temperature of the mixed solution after high-temperature refining to be below 170 ℃, quickly heating the mixed solution to 170-200 ℃, and keeping the temperature for a period of time;
s5: and (5) when the temperature of the mixed solution obtained in the step (S4) is reduced to be below 80 ℃, homogenizing and degassing the mixed solution to obtain the composite barium-based lubricating grease.
Preferably, the modified tungsten disulfide powder is iron-loaded graphene-based tungsten disulfide nano powder, and the iron-loaded graphene-based tungsten disulfide nano powder is prepared by the following method, and the method comprises the following steps:
s1: respectively adding a water-soluble tungsten source and a water-soluble sulfur source into water to dissolve the tungsten source and the water-soluble sulfur source to form a tungsten source aqueous solution and a sulfur source aqueous solution, mixing the tungsten source aqueous solution and the sulfur source aqueous solution according to a certain proportion, and adjusting the mixed solution to be acidic by using a strong acid solution;
s2: adding graphene oxide into the solution obtained in the step S1, and performing ultrasonic treatment to obtain a first suspension;
s3: reacting the first suspension obtained in the step S2 at the temperature of 170-200 ℃ and under the pressure of 2-4 MPa;
s4: cooling the reaction liquid after the reaction in the step S3, centrifuging and washing, and freeze-drying the centrifuged and washed matter to obtain the graphene oxide-based tungsten disulfide composite nano material;
s5: adding the graphene oxide-based tungsten disulfide composite nano material obtained in the step S4 into a soluble iron salt solution, and performing ultrasonic treatment to obtain a second suspension;
s6: heating the second suspension obtained in the step S5 to 80-100 ℃, adding a strong base solution under stirring to adjust the mixed solution to be neutral or alkaline, and performing reflux reaction;
s7: and cooling the reaction liquid after the reaction in the step S6, performing centrifugal washing and drying, and finally heating the dried product to 300-400 ℃ under the protection of nitrogen for calcining to obtain the iron-loaded graphene-based tungsten disulfide nano powder.
Preferably, in step S1, the pH of the mixed solution is adjusted to 1 to 3 by using a strong acid solution, wherein the strong acid is preferably one of hydrochloric acid, sulfuric acid and nitric acid; in the step S6, adding a strong alkali solution to adjust the pH of the mixed solution to 7-10, wherein the strong alkali is preferably potassium hydroxide or sodium hydroxide.
Preferably, the concentration of the tungsten source water solution is 36-54g/L, the concentration of the sulfur source water solution is 16-32g/L, and the volume ratio of the tungsten source water solution to the sulfur source water solution is 1: 1-3.
Preferably, the mass of the graphene oxide added in step S2 is 5wt% to 10wt% of the total mass of the tungsten source, the sulfur source and the graphene oxide.
Preferably, the concentration of iron ions in the soluble iron salt solution is 3-5 mg/mL, and the mass ratio of the mass of the iron ions in the soluble iron salt solution to the mass of the graphene oxide-based tungsten disulfide composite nano material obtained in the step S4 is 6-10: 1.
Preferably, the water-soluble sulfur source is at least one of thiourea, sodium thiosulfate, sodium sulfide and thioacetamide, the water-soluble tungsten source is preferably at least one of sodium tungstate and ammonium tungstate, and the soluble iron salt is preferably at least one of ferric nitrate, ferric sulfate and ferric chloride.
Preferably, the ultrasonic processing conditions in step S2 and step S5 are: the processing frequency is 20-22 kHz, the processing power is 200-220W, and the processing time is 20-40 min.
Preferably, the temperature rising manner in the step S7 is temperature programming, and the temperature programming rate is 3 to 5 ℃/min.
Preferably, the reaction time in the step S3 is 18-36 hours, the reaction time in the step S6 is preferably 2-4 hours, and the calcination time in the step S7 is preferably 1-2 hours.
Preferably, the composite barium-based lubricating grease comprises the following components in parts by weight: 60-70 parts of base oil, 10-15 parts of fatty acid, 8-12 parts of barium hydroxide octahydrate and 4-8 parts of iron-loaded graphene-based tungsten disulfide.
Preferably, the fatty acid is 12-hydroxystearic acid, the base oil is preferably a mineral base oil and/or a synthetic base oil, the synthetic base oil is preferably at least one of a synthetic hydrocarbon, preferably at least one of an ethylene oligomer, a propylene oligomer, polybutene, polyisobutylene, polyalphaolefin, polylefin and halogenated products of the above synthetic hydrocarbon, an alkyl aromatic hydrocarbon, preferably at least one of alkylbenzene, alkyl naphthalene and alkyl aromatic hydrocarbon containing a hetero atom, a synthetic ester, preferably at least one of a monoester, a diester, a polyol ester, a polymer ester, a carbonate, a phosphate, a citrate, a silicate and an olefin-acrylate copolymer, an alkyl aromatic hydrocarbon, a synthetic ester is preferably at least one of an aliphatic polyether, a polyether-acrylate copolymer, a polyether is preferably at least one of a mineral base oil and/or a synthetic base oil, the synthetic base oil is preferably at least one of a synthetic hydrocarbon, an alkyl aromatic hydrocarbon, a synthetic ester, a polyether, a halogenated hydrocarbon, a poly-olefin, a poly-alpha-olefin, a poly-olefin, and a poly-olefin, a poly-one, and a poly-one, At least one of polyphenyl ether, polysulfide and perfluoroalkyl polyether, the polysiloxane is preferably at least one of dipolymer siloxane, tripolymer siloxane, tetrapolysiloxane, octapolysiloxane and cyclic polytetrasiloxane, and the small molecular organic acid is preferably one or more of glutaric acid, suberic acid, sebacic acid, citric acid and malic acid.
Preferably, the saponification reaction time in the step S1 is 1.5-2.5 hours, the constant-temperature stirring time in the step S2 is 0.5-1.5 hours, the high-temperature refining time in the step S2 is 1.5-2.5 hours, and the constant-temperature time in the step S4 is 20-40 minutes.
The invention also provides the composite barium-based lubricating grease prepared by the method.
The beneficial effects of the invention are:
fatty acid, base oil and barium hydroxide octahydrate are subjected to saponification reaction, then the temperature is raised, small molecular organic acid and tungsten disulfide powder or modified tungsten disulfide powder are added and stirred at constant temperature, then high-temperature refining is carried out, then the temperature is reduced, the temperature is rapidly raised and lowered again at constant temperature, and finally the mixed solution is homogenized and degassed to obtain the composite barium-based lubricating grease; particularly, the iron-loaded graphene-based tungsten disulfide nano powder can further improve the extreme pressure wear resistance, high temperature resistance, thickening performance, oxidation resistance and water spray resistance of the composite barium-based lubricating grease, and when the composite barium-based lubricating grease is used on parts such as bearings for a long time, the iron-loaded graphene-based tungsten disulfide nano powder is not easy to agglomerate on the surfaces of the parts such as bearings.
(2) The preparation method of the composite barium-based lubricating grease is simple, convenient and controllable, is suitable for amplification, has lower experimental environment requirements and small pollution to the environment, and can reduce the harm to operators when toxic substances participate.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The technical solution of the present application will be described in detail with reference to the following examples.
Example 1
The embodiment provides a preparation method of iron-loaded graphene-based tungsten disulfide nano powder, which comprises the following steps:
s1: respectively adding sodium tungstate and thioacetamide into deionized water to be fully dissolved to form a sodium tungstate aqueous solution with a tungsten concentration of 40g/L and a thioacetamide aqueous solution with a sulfur concentration of 32g/L, mixing 0.1L of the sodium tungstate aqueous solution with 0.1L of the thioacetamide aqueous solution, and adjusting the pH value of the mixed solution to 1 by using a hydrochloric acid aqueous solution;
s2: adding 0.8g of graphene oxide into the solution obtained in the step S1, and carrying out ultrasonic treatment for 30min under the conditions that the frequency is 20kHz and the power is 200W to obtain a first suspension;
s3: transferring the first suspension obtained in the step S2 to a 100mL polytetrafluoroethylene high-pressure reaction kettle, moving the reaction kettle to a heating box, and reacting for 36 hours at the temperature of 200 ℃ and the pressure of 3 MPa;
s4: cooling the reaction solution obtained after the reaction in the step S3 to room temperature, centrifugally washing for 4-6 times, and freeze-drying the centrifugally washed matter to obtain the graphene oxide-based tungsten disulfide composite nano material;
s5: adding 50mg of the graphene oxide-based tungsten disulfide composite nano material obtained in the step S4 into 100mL of ferric nitrate solution (the concentration of iron ions is 5 mg/mL), and carrying out ultrasonic treatment for 30min under the conditions that the frequency is 22kHz and the power is 220W to obtain second suspension;
s6: transferring the second suspension obtained in the step S5 to an oil bath pot, heating to 100 ℃, adding NaOH aqueous solution under the stirring condition to adjust the pH of the mixed solution to 7, and keeping the temperature to perform reflux reaction for 4 hours;
s7: and (4) cooling the reaction liquid after the reaction of the step S6, centrifugally washing for 4-6 times, drying for 36h in a vacuum drying oven, and finally transferring the dried product to a tubular furnace, and calcining for 2 h at the temperature of 300 ℃ by temperature programming (the temperature rising rate is 5 ℃/min) under the protection of nitrogen gas to obtain the iron-loaded graphene-based tungsten disulfide nano powder.
Example 2
The embodiment provides a preparation method of iron-loaded graphene-based tungsten disulfide nano powder, which comprises the following steps:
s1: respectively adding sodium tungstate and thioacetamide into deionized water to be fully dissolved to form a sodium tungstate aqueous solution with the tungsten concentration of 36g/L and a thioacetamide aqueous solution with the sulfur concentration of 30g/L, then mixing 0.2L of the sodium tungstate aqueous solution with 0.2L of the thioacetamide aqueous solution, and adjusting the pH value of the mixed solution to 1 by using a hydrochloric acid aqueous solution;
s2: adding 0.7g of graphene oxide and graphene oxide into the solution obtained in the step S1, and carrying out ultrasonic treatment for 30min under the conditions that the frequency is 20kHz and the power is 200W to obtain a first suspension;
s3: transferring the first suspension obtained in the step S2 to a 100mL polytetrafluoroethylene high-pressure reaction kettle, transferring the reaction kettle to a heating box, and reacting for 36 hours at the temperature of 180 ℃ and the pressure of 2 MPa;
s4: cooling the reaction liquid obtained after the reaction in the step S3 to room temperature, centrifugally washing for 4-6 times, and freeze-drying the centrifugally washed matter to obtain the graphene oxide-based tungsten disulfide composite nano material;
s5: adding 50mg of the graphene oxide-based tungsten disulfide composite nano material obtained in the step S4 into 100mL of ferric nitrate solution (the concentration of iron ions is 5 mg/mL), and carrying out ultrasonic treatment for 30min under the conditions that the frequency is 22kHz and the power is 220W to obtain second suspension;
s6: transferring the second suspension obtained in the step S5 to an oil bath pan, heating to 100 ℃, adding a KOH aqueous solution under the stirring condition to adjust the pH of the mixed solution to 10, and maintaining the temperature to perform reflux reaction for 4 hours;
s7: and (4) cooling the reaction liquid after the reaction of the step S6, centrifugally washing for 4-6 times, drying for 36h in a vacuum drying oven, and finally transferring the dried product to a tubular furnace, and calcining for 1 h at the temperature of 400 ℃ by temperature programming (the temperature rise rate is 5 ℃/min) under the protection of nitrogen gas to obtain the iron-loaded graphene-based tungsten disulfide nano powder.
Example 3
The embodiment provides a preparation method of iron-loaded graphene-based tungsten disulfide nano powder, which comprises the following steps:
s1: respectively adding ammonium tungstate and sodium sulfide into deionized water, fully dissolving to form an ammonium tungstate aqueous solution with a tungsten concentration of 54g/L and a sodium sulfide aqueous solution with a sulfur concentration of 30g/L, mixing 0.12L of the ammonium tungstate aqueous solution with 0.24L of the sodium sulfide aqueous solution, and adjusting the pH value of the mixed solution to 2 by using a nitric acid aqueous solution;
s2: adding 1.2g of graphene oxide into the solution obtained in the step S1, and carrying out ultrasonic treatment for 20min under the conditions that the frequency is 20kHz and the power is 200W to obtain a first suspension;
s3: transferring the first suspension obtained in the step S2 to a 100mL polytetrafluoroethylene high-pressure reaction kettle, transferring the reaction kettle to a heating box, and reacting for 36 hours at the temperature of 170 ℃ and the pressure of 4 MPa;
s4: cooling the reaction liquid obtained after the reaction in the step S3 to room temperature, centrifugally washing for 4-6 times, and freeze-drying the centrifugally washed matter to obtain the graphene oxide-based tungsten disulfide composite nano material;
s5: adding 50mg of the graphene oxide-based tungsten disulfide composite nano material obtained in the step S4 into 100mL of ferric nitrate solution (the concentration of ferric ions is 5 mg/mL), and performing ultrasonic treatment for 30min under the conditions that the frequency is 22kHz and the power is 220W to obtain a second suspension;
s6: transferring the second suspension obtained in the step S5 to an oil bath pan, heating to 100 ℃, adding NaOH aqueous solution under stirring to adjust the pH of the mixed solution to 8, keeping the temperature, and carrying out reflux reaction for 2 hours;
s7: and cooling the reaction liquid after the reaction of the step S6, centrifugally washing for 4-6 times, drying for 36h in a vacuum drying oven, and finally transferring the dried product into a tubular furnace, and calcining for 1.5 h at the temperature of 400 ℃ under the protection of nitrogen by temperature programming (the heating rate is 3 ℃/min) to obtain the iron-loaded graphene-based tungsten disulfide nano powder.
Example 4
The embodiment provides a preparation method of iron-loaded graphene-based tungsten disulfide nano powder, which comprises the following steps:
s1: respectively adding ammonium tungstate and sodium thiosulfate into deionized water, fully dissolving to form an ammonium tungstate aqueous solution with the concentration of 42g/L and a sodium thiosulfate aqueous solution with the concentration of 16g/L, mixing 0.05L of the ammonium tungstate aqueous solution and 0.15L of the sodium thiosulfate aqueous solution, and adjusting the pH value of the mixed solution to 2 by using a nitric acid aqueous solution;
s2: adding 0.5g of graphene oxide into the solution obtained in the step S1, and carrying out ultrasonic treatment for 25min under the conditions that the frequency is 20kHz and the power is 200W to obtain a first suspension;
s3: transferring the first suspension obtained in the step S2 to a 100mL polytetrafluoroethylene high-pressure reaction kettle, transferring the reaction kettle to a heating box, and reacting for 18 hours at the temperature of 200 ℃ and the pressure of 3 MPa;
s4: cooling the reaction solution obtained after the reaction in the step S3 to room temperature, centrifugally washing for 4-6 times, and freeze-drying the centrifugally washed matter to obtain the graphene oxide-based tungsten disulfide composite nano material;
s5: adding 50mg of the graphene oxide-based tungsten disulfide composite nano material obtained in the step S4 into 100mL of ferric nitrate solution (the concentration of iron ions is 3 mg/mL), and carrying out ultrasonic treatment for 30min under the conditions that the frequency is 22kHz and the power is 220W to obtain second suspension;
s6: transferring the second suspension obtained in the step S5 to an oil bath pot, heating to 80 ℃, adding NaOH aqueous solution under the stirring condition to adjust the pH of the mixed solution to 8, and keeping the temperature to perform reflux reaction for 4 hours;
s7: and cooling the reaction liquid after the reaction of the step S6, centrifugally washing for 4-6 times, drying for 36h in a vacuum drying oven, and finally transferring the dried product into a tubular furnace, and calcining for 2 h at the temperature of 400 ℃ under the protection of nitrogen by temperature programming (the heating rate is 5 ℃/min) to obtain the iron-loaded graphene-based tungsten disulfide nano powder.
Example 5
A preparation method of composite barium-based lubricating grease comprises the following components in parts by weight: 65 parts of base oil, 12 parts of stearic acid, 10 parts of barium hydroxide octahydrate and 6 parts of modified molybdenum disulfide powder, wherein the composite barium-based lubricating grease is prepared by the following steps:
s1: mixing and heating 12-hydroxy fatty acid and citric acid ester base oil with the mass of A, adding citric acid ester base oil with the mass of B and barium hydroxide octahydrate when the temperature of mixed liquid is raised to 110 ℃, and carrying out saponification for 2 hours, wherein the ratio of the mass of A to the mass of B is 1: 2;
s2: gradually heating the reaction solution after the saponification reaction to 130 ℃, exhausting water vapor, adding suberic acid and the iron-loaded graphene-based tungsten disulfide nanopowder prepared in example 1, and stirring at constant temperature for 1 hour;
s3: heating the mixed solution obtained in the step S2 to 180 ℃, and refining at high temperature for 2 hours;
s4: reducing the temperature of the mixed solution after high-temperature refining to below 170 ℃, quickly heating the mixed solution to 200 ℃, and keeping the temperature for 30 minutes;
s5: and (5) when the temperature of the mixed liquid obtained in the step (S4) is reduced to be below 80 ℃, pumping the mixed liquid into a high-pressure homogenizer for homogenization, and then degassing to obtain the composite barium-based lubricating grease.
Example 6
A preparation method of composite barium-based lubricating grease comprises the following components in parts by weight: 60 parts of base oil, 15 parts of stearic acid, 8 parts of barium hydroxide octahydrate and 8 parts of modified molybdenum disulfide powder, wherein the composite barium-based lubricating grease is prepared by the following steps:
s1: mixing and heating 12-hydroxy fatty acid and base oil with the mass of A, adding the base oil with the mass of B and barium hydroxide octahydrate when the temperature of a mixed solution rises to 110 ℃, and carrying out saponification for 2 hours, wherein the base oil comprises citrate base oil and poly alpha-olefin base oil with the mass ratio of 1:1, and the ratio of the mass of A to the mass of B is 1: 1.5;
s2: gradually heating the reaction solution after the saponification reaction to 130 ℃, exhausting water, adding citric acid and the iron-loaded graphene-based tungsten disulfide nano powder prepared in the example 2, and stirring at constant temperature for 0.5 hour;
s3: heating the mixed solution obtained in the step S2 to 180 ℃, and refining at high temperature for 2 hours;
s4: reducing the temperature of the mixed solution after high-temperature refining to below 170 ℃, quickly heating the mixed solution to 200 ℃, and keeping the temperature for 30 minutes;
s5: and (5) when the temperature of the mixed liquid obtained in the step (S4) is reduced to be below 80 ℃, pumping the mixed liquid into a high-pressure homogenizer for homogenization, and then degassing to obtain the composite barium-based lubricating grease.
Example 7
A preparation method of composite barium-based lubricating grease comprises the following components in parts by weight: 70 parts of base oil, 10 parts of stearic acid, 12 parts of barium hydroxide octahydrate and 4 parts of modified molybdenum disulfide powder, wherein the preparation steps of the composite barium-based lubricating grease are as follows:
s1: mixing and heating 12-hydroxy fatty acid and base oil with the mass of A, adding the base oil with the mass of B and barium hydroxide octahydrate when the temperature of the mixed solution rises to 100 ℃, and carrying out saponification for 2.5 hours, wherein the base oil comprises carbonate base oil and mineral base oil Ib150 with the mass ratio of 1:1, and the ratio of the mass of A to the mass of B is 1: 2.5;
s2: gradually heating the reaction solution after the saponification reaction to 120 ℃, exhausting water vapor, adding citric acid and glutaric acid in a volume ratio of 1:1, adding the iron-loaded graphene-based tungsten disulfide nano powder prepared in the example 3, and stirring at constant temperature for 1.5 hours;
s3: heating the mixed solution obtained in the step S2 to 200 ℃, and refining at high temperature for 1.5 hours;
s4: reducing the temperature of the mixed solution after high-temperature refining to below 170 ℃, quickly heating the mixed solution to 200 ℃, and keeping the temperature for 20 minutes;
s5: and (5) when the temperature of the mixed liquid obtained in the step (S4) is reduced to be below 80 ℃, pumping the mixed liquid into a high-pressure homogenizer for homogenization, and then degassing to obtain the composite barium-based lubricating grease.
Example 8
A preparation method of composite barium-based lubricating grease comprises the following components in parts by weight: 63 parts of base oil, 12 parts of stearic acid, 10 parts of barium hydroxide octahydrate and 6 parts of modified molybdenum disulfide powder, wherein the composite barium-based lubricating grease is prepared by the following steps:
s1: mixing and heating 12-hydroxy fatty acid and base oil with the mass of A, adding base oil with the mass of B and barium hydroxide octahydrate when the temperature of a mixed solution is raised to 105 ℃, and carrying out saponification reaction for 2 hours, wherein the base oil comprises polyisobutylene base oil and mineral base oil Ib150 with the mass ratio of 1:1, and the ratio of the mass composite barium-based lubricating grease A to the mass B is 1: 2;
s2: gradually heating the reaction solution after the saponification reaction to 125 ℃, exhausting water vapor, adding suberic acid and the iron-loaded graphene-based tungsten disulfide nanopowder prepared in example 4, and stirring at constant temperature for 1.5 hours;
s3: heating the mixed solution obtained in the step S2 to 170 ℃, and refining at high temperature for 2.5 hours;
s4: reducing the temperature of the mixed solution after high-temperature refining to be below 150 ℃, quickly heating the mixed solution to 170 ℃, and keeping the temperature for 40 minutes;
s5: and (5) when the temperature of the mixed liquid obtained in the step (S4) is reduced to be below 80 ℃, pumping the mixed liquid into a high-pressure homogenizer for homogenization, and degassing to obtain the composite barium-based lubricating grease.
Example 9
This example differs from example 5 only in that: the iron-loaded graphene-based tungsten disulfide nanopowder of example 5 was changed to a common molybdenum disulfide powder.
Example 10
This example differs from example 6 only in that: the iron-loaded graphene-based tungsten disulfide nanopowder of example 6 was changed to a common molybdenum disulfide powder.
Example 11
This example differs from example 7 only in that: the iron-loaded graphene-based tungsten disulfide nanopowder of example 7 was changed to a common molybdenum disulfide powder.
Example 12
This example differs from example 8 only in that: the iron-loaded graphene-based tungsten disulfide nanopowder of example 8 was changed to a common molybdenum disulfide powder.
Effects of the invention
The effect example tests the wide temperature drop point (test method: GB/T3498-2008), the working cone penetration (test method: GB/T269-91), the similar viscosity (test method: SH/T0048-1991), the oxidation stability (test method: SH/T0325-2004), the water content (test method: GB/T512-1990), the water leaching loss (test method: SH/T0109-2004), and the friction coefficient (test method: SH-T0847-NB 2010) of the composite barium-based lubricating grease prepared in the examples 5-9, and the results show that the water content of the composite barium-based lubricating grease prepared in the examples 5-9 is less than 0.1%, see Table 1.
TABLE 1 results of performance testing of greases prepared in examples 5-9
Figure DEST_PATH_IMAGE001
It will be appreciated by those skilled in the art that the higher the wide temperature drop point, the better the high temperature resistance of the grease; the smaller the working cone penetration, the better the thickening performance of the lubricating grease; the smaller the similar viscosity is, the smaller the friction loss is, the smaller the oxidation stability is, and the better the oxidation resistance of the lubricating grease is; the smaller the water spray loss is, the better the water spray resistance is; the smaller the friction coefficient, the better the antifriction properties of the grease.
Comparing the performance of the barium-based composite greases prepared in examples 5-8 and 9-12, it can be seen that the greases of the present invention have better high temperature resistance, thickening performance, oxidation resistance, water spray resistance and antifriction performance by using the iron-loaded graphene-based tungsten disulfide nanopowder.
In light of the foregoing description of the preferred embodiments according to the present application, it is to be understood that various changes and modifications may be made without departing from the spirit and scope of the invention. The technical scope of the present application is not limited to the contents of the specification, and must be determined according to the scope of the claims.

Claims (31)

1. The preparation method of the composite barium-based lubricating grease is characterized by comprising the following steps of:
s1: mixing and heating fatty acid and base oil with the mass A, adding the base oil with the mass B and barium hydroxide octahydrate for saponification reaction when the temperature of the mixed solution is raised to 100-110 ℃, wherein the ratio of the mass A to the mass B is 1: 1.5-2.5;
s2: gradually heating the reaction solution after the saponification reaction to 120-130 ℃, exhausting water, adding a small molecular organic acid and graphene-based tungsten disulfide nano powder loaded with iron, and stirring at constant temperature;
s3: heating the mixed solution obtained in the step S2 to 170-200 ℃, and refining at a high temperature;
s4: reducing the temperature of the mixed solution after high-temperature refining to be below 170 ℃, quickly heating the mixed solution to 170-200 ℃, and keeping the temperature for a period of time;
s5: when the temperature of the mixed liquid obtained in the step S4 is reduced to be below 80 ℃, homogenizing and degassing the mixed liquid to obtain the composite barium-based lubricating grease;
the iron-loaded graphene-based tungsten disulfide nano powder is prepared by the following method, and comprises the following steps:
s1: respectively adding a water-soluble tungsten source and a water-soluble sulfur source into water to dissolve the tungsten source and the sulfur source to form a tungsten source aqueous solution and a sulfur source aqueous solution, mixing the tungsten source aqueous solution and the sulfur source aqueous solution according to a certain proportion, and adjusting the mixed solution to be acidic by using a strong acid solution;
s2: adding graphene oxide into the solution obtained in the step S1, and performing ultrasonic treatment to obtain a first suspension;
s3: reacting the first suspension obtained in the step S2 at the temperature of 170-200 ℃ and under the pressure of 2-4 MPa;
s4: cooling the reaction liquid after the reaction in the step S3, centrifuging and washing, and freeze-drying the centrifuged and washed matter to obtain the graphene oxide-based tungsten disulfide composite nano material;
s5: adding the graphene oxide-based tungsten disulfide composite nano material obtained in the step S4 into a soluble iron salt solution, and performing ultrasonic treatment to obtain a second suspension;
s6: heating the second suspension obtained in the step S5 to 80-100 ℃, adding a strong base solution under a stirring condition to adjust the mixed solution to be neutral or alkaline, and carrying out a reflux reaction;
s7: and cooling the reaction liquid after the reaction in the step S6, performing centrifugal washing and drying, and finally heating the dried product to 300-400 ℃ under the protection of nitrogen for calcining to obtain the iron-loaded graphene-based tungsten disulfide nano powder.
2. The method for preparing the composite barium-based lubricating grease according to claim 1, wherein the composite barium-based lubricating grease comprises the following components in parts by weight: 60-70 parts of base oil, 10-15 parts of fatty acid, 8-12 parts of barium hydroxide octahydrate and 4-8 parts of iron-loaded graphene-based tungsten disulfide.
3. The method for preparing the barium complex grease as claimed in claim 1 or 2, wherein the fatty acid is 12-hydroxystearic acid.
4. The method for preparing the composite barium-based grease according to claim 1 or 2, wherein the base oil is a mineral base oil and/or a synthetic base oil.
5. The method for preparing the composite barium-based grease of claim 4, wherein the synthetic base oil is at least one of synthetic hydrocarbon, synthetic ester, polyether, halogenated hydrocarbon, polysiloxane and fluorine-containing oil.
6. The method for preparing the barium complex grease as claimed in claim 5, wherein the synthetic hydrocarbon is at least one of polyisobutylene, polyalphaolefin and polyinternal olefin.
7. The method for preparing the barium-based composite grease according to claim 5, wherein the synthetic hydrocarbon is an alkyl aromatic hydrocarbon, and the alkyl aromatic hydrocarbon is at least one of an alkylbenzene, an alkyl naphthalene, and an alkyl aromatic hydrocarbon containing a heteroatom.
8. The method for preparing the barium-based composite grease according to claim 5, wherein the synthetic ester is at least one of a monoester, a diester, a polyol ester, a polymer ester, a carbonate, a phosphate, a citrate and a silicate.
9. The method for preparing the barium-based composite grease according to claim 5, wherein the polyether is at least one of aliphatic polyether, polyphenylene oxide, polysulfide and perfluoroalkyl polyether.
10. The method of preparing the barium-based composite grease according to claim 5, wherein the polysiloxane is at least one of a disiloxane, a trisiloxane, a tetrapolysiloxane, an octapolysiloxane, and a cyclotetrasiloxane.
11. The method for preparing the barium complex grease as claimed in claim 1, wherein the small molecular organic acid is one or more of glutaric acid, suberic acid, sebacic acid, citric acid and malic acid.
12. The method for preparing the composite barium-based grease of claim 1 or 2, wherein the saponification reaction time in step S1 is 1.5-2.5 hours.
13. The method for preparing the composite barium-based grease according to claim 1 or 2, wherein the stirring time at constant temperature in step S2 is 0.5-1.5 hours.
14. The method for preparing the barium complex grease of claim 1 or 2, wherein the refining time at high temperature in step S3 is 1.5-2.5 hours.
15. The method for preparing the composite barium-based grease lubricant according to claim 1 or 2, wherein the constant temperature is maintained in step S4 for 20-40 minutes.
16. The method for preparing the composite barium-based grease according to claim 1, wherein in the step of preparing the iron-loaded graphene-based tungsten disulfide nanopowder, in step S1, the pH of the mixed solution is adjusted to 1-3 by using a strong acid solution.
17. The method for preparing the barium-based composite grease of claim 1, wherein the strong acid is one of hydrochloric acid, sulfuric acid and nitric acid.
18. The method for preparing the composite barium-based grease according to claim 1, wherein in the step of preparing the iron-loaded graphene-based tungsten disulfide nanopowder, in step S6, a strong alkali solution is added to adjust the pH of the mixed solution to 7-10.
19. The method for preparing the composite barium-based grease as claimed in claim 1, wherein the strong base is potassium hydroxide or sodium hydroxide.
20. The preparation method of the composite barium-based lubricating grease of claim 1, wherein the concentration of the tungsten source aqueous solution is 36-54g/L, the concentration of the sulfur source aqueous solution is 16-32g/L, and the volume ratio of the tungsten source aqueous solution to the sulfur source water solution is 1: 1-3.
21. The method for preparing the composite barium-based grease lubricant according to claim 1, wherein the mass of the graphene oxide added in the step S2 accounts for 5wt% -10wt% of the total mass of the tungsten source, the sulfur source and the graphene oxide.
22. The method for preparing the composite barium-based lubricating grease according to claim 1, wherein the concentration of iron ions in the soluble iron salt solution is 3-5 mg/mL.
23. The preparation method of the composite barium-based lubricating grease as claimed in claim 1, wherein the mass ratio of the mass of iron ions in the soluble iron salt solution to the mass of the graphene oxide-based tungsten disulfide composite nano material obtained in step S4 is 6-10: 1.
24. The method for preparing the composite barium-based grease of claim 1, wherein the water-soluble sulfur source is at least one of thiourea, sodium thiosulfate, sodium sulfide and thioacetamide.
25. The method for preparing the barium complex grease as claimed in claim 1, wherein the water-soluble tungsten source is at least one of sodium tungstate and ammonium tungstate.
26. The method for preparing the barium complex grease as claimed in claim 1, wherein the soluble ferric salt is at least one of ferric nitrate, ferric sulfate and ferric chloride.
27. The method for preparing the composite barium-based grease of claim 1, wherein the temperature raising manner of step S7 is temperature programming, and the temperature programming rate is 3-5 ℃/min.
28. The method for preparing the composite barium-based grease lubricant according to claim 1, wherein in the method for preparing the iron-loaded graphene-based tungsten disulfide nano powder, the reaction time in the step S3 is 18-36 hours.
29. The method for preparing the composite barium-based lubricating grease according to claim 1, wherein in the method for preparing the iron-loaded graphene-based tungsten disulfide nano powder, the reaction time in step S6 is 2-4 hours.
30. The method for preparing the composite barium-based grease lubricant according to claim 1, wherein in the method for preparing the iron-loaded graphene-based tungsten disulfide nano powder, the calcination time in step S7 is 1-2 hours.
31. A barium complex grease prepared by the method of any one of claims 1 to 30.
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