CN113604267A - High-rotation-speed spinning spindle lubricating grease composition and preparation method and application thereof - Google Patents

High-rotation-speed spinning spindle lubricating grease composition and preparation method and application thereof Download PDF

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Publication number
CN113604267A
CN113604267A CN202110936633.3A CN202110936633A CN113604267A CN 113604267 A CN113604267 A CN 113604267A CN 202110936633 A CN202110936633 A CN 202110936633A CN 113604267 A CN113604267 A CN 113604267A
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base oil
grease composition
lubricating grease
ethylene propylene
mass ratio
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CN113604267B (en
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高峰
张晓凯
包锐
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China Petroleum and Chemical Corp
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China Petroleum and Chemical Corp
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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
    • 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
    • C10M2203/102—Aliphatic fractions
    • C10M2203/1025—Aliphatic fractions used as base material
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    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/0206—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers used as base material
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    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/022—Ethene
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    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/024—Propene
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02—Hydroxy compounds
    • C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/026—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
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    • 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
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    • 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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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/16—Naphthenic acids
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    • 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
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/06—Thio-acids; Thiocyanates; Derivatives thereof
    • C10M2219/062—Thio-acids; Thiocyanates; Derivatives thereof having carbon-to-sulfur double bonds
    • C10M2219/066—Thiocarbamic type compounds
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    • 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
    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
    • C10M2223/043—Ammonium or amine salts thereof
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    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
    • C10M2223/045—Metal containing thio derivatives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
    • C10M2223/047—Thioderivatives not containing metallic elements
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/06—Organic compounds derived from inorganic acids or metal salts
    • C10M2227/061—Esters derived from boron
    • C—CHEMISTRY; METALLURGY
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    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/02—Pour-point; Viscosity index
    • C—CHEMISTRY; METALLURGY
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    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/10—Inhibition of oxidation, e.g. anti-oxidants
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
    • C—CHEMISTRY; METALLURGY
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    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/76—Reduction of noise, shudder, or vibrations
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Semi-solids; greasy

Abstract

The invention relates to the technical field of lubricating grease, and particularly relates to a lubricating grease composition for a high-rotation-speed spinning spindle, and a preparation method and application thereof. The invention provides a lubricating grease composition which is prepared from the following raw materials: thickening agent, base oil, extreme pressure antiwear agent and structure improver, wherein the structure improver is one or a mixture of two of ethylene propylene rubber and ethylene propylene diene monomer, and the kinematic viscosity of the base oil at 40 ℃ is 200-600mm2And/s, the mass ratio of the structure improver to the base oil is (0.01-0.05): 1. the lubricating grease composition provided by the invention has good adhesion performance and excellent anti-friction and anti-vibration performance, can effectively reduce friction resistance, reduce vibration and noise and save power consumption; the lubricating grease also has good mechanical stability and colloid stability, can ensure that the spinning spindle can stably and effectively run at high rotating speed without loss, and can be used for lubricating the spinning spindle at high rotating speed.

Description

High-rotation-speed spinning spindle lubricating grease composition and preparation method and application thereof
Technical Field
The invention relates to the technical field of lubricating grease, and particularly relates to a lubricating grease composition for a high-rotation-speed spinning spindle, and a preparation method and application thereof.
Background
The spindle is used as a symbol of the textile industry, and the equipment scale of a spinning mill is usually measured by the number of the spindles, which is enough to indicate the importance of the spindle to the textile industry. The spinning spindle is used as the main twisting winding part of the spinning frame, is a high-speed rotating part, consists of more than 20 parts, and comprises a positioning ring, a spindle bottom supporting sheet, a spindle rod, a spindle foot, a spindle disc, a yarn cutter blade, a yarn cutter positioning sheet, an aluminum sleeve, a vibration absorption coil spring, a supporting sheet, a bearing cover, a bearing seat, an elastic tube and the like.
The high-speed operation of the cotton spinning spindle is the key for realizing high benefit in the textile industry, and the quality of the operation condition directly influences the yield and the quality of textile products. However, due to the structural characteristics of the spindle, the cotton spinning spindle has the problems of increased power consumption and higher noise when spinning at high speed, and the key problem to be solved is vibration. The negative effects of vibration are significant and the sources of noise, power consumption, etc. problems are all due to the effect of vibration on the cotton spinning spindle.
When the rotating speed of the traditional spinning spindle is below 20000 revolutions per minute, the spinning spindle can normally run without adopting a lubricant. However, when the rotation speed is increased to over 20000 rpm, the vibration of the spindle is caused by the resonance generated by the vibration of the whole vehicle, and the relative vibration friction between the inner container and the spindle foot causes noise and even abrasion. In order to accelerate the automatic and high-speed production process of the textile industry and match the automatic shakeout machine and the spinning frame for collective doffing transformation, the problems of vibration and noise of the spindle in a high-speed state need to be solved, so that the spindle lubricating grease meeting the high-speed energy-saving requirement of the textile spindle has important significance.
Due to the special working condition of the spinning spindle at high speed, the lubricating grease is required to have good extreme pressure abrasion resistance so as to ensure the working stability of the spindle under high-frequency vibration; the good service life ensures the long-term effective operation of the spindle; excellent mechanical stability and colloid stability, and can prevent the lubricating grease from becoming thin and the oil content from increasing due to the high-speed operation of the spindle, so that the lubricating grease can be prevented from being lost and polluting cotton yarns.
At present, no special lubricating grease for high-speed spinning spindles exists in the prior art, great inconvenience is brought to type selection of the lubricating grease for the high-speed spinning spindles, vibration and noise of the spindles are large due to improper type selection, abrasion is serious, and meanwhile, machine tool stopping is forced due to grease loss, so that a great amount of economic loss is caused. Therefore, it is necessary to develop a special grease for high-speed spinning spindles.
Disclosure of Invention
The invention aims to provide a lubricating grease composition. The lubricating grease composition can meet the special working condition requirements of high-speed spinning spindles. The invention also provides a preparation method and application of the lubricating grease composition.
Aiming at the special working condition of the high-speed spinning spindle during high-speed operation, the lubricating grease composition can be suitable for the high-speed spinning spindle by optimizing the formula of the lubricating grease composition, and the problems of noise, vibration and abrasion of the high-speed spinning spindle and the loss of the lubricating grease in the using process are solved. In the research and development process, the invention discovers that the ethylene propylene rubber, the ethylene propylene diene monomer and the base oil can be well matched by adding the ethylene propylene rubber and the ethylene propylene diene monomer and adaptively optimizing the formula of the base oil, so that the mechanical stability and the colloid stability of the lubricating grease are obviously improved.
Specifically, the invention provides the following technical scheme:
the invention provides a lubricating grease composition which is prepared from the following raw materials: thickening agent, base oil, extreme pressure antiwear agent and structure improver,
wherein the structure improver is one or a mixture of two of ethylene propylene rubber and ethylene propylene diene monomer,
the kinematic viscosity at 40 ℃ of the base oil is 200-2/s，
The mass ratio of the structure improver to the base oil is (0.01-0.05): 1.
preferably, the kinematic viscosity at 40 ℃ of the base oil is 350-600mm2/s。
The invention discovers that the PAO synthetic oil and the 150BS base oil with specific proportions can enable the structure modifier, the base oil and the thickening agent to better cooperate with each other in the base oil meeting the performances, and the mechanical stability and the colloid stability of the lubricating grease are obviously improved.
Preferably, the base oil is a mixture of base oil and base oil in a mass ratio of 1: the PAO synthetic oil of (1-5) and 150BS base oil.
And for the structure improver, when the structure improver is a mixture of ethylene propylene rubber and ethylene propylene diene monomer, the mass ratio of the ethylene propylene rubber to the ethylene propylene diene monomer is (0.5-2): 1.
specifically, the preparation raw materials of the lubricating grease composition comprise the following components in parts by weight: 5-10 parts of thickening agent, 60-80 parts of base oil, 0.5-5 parts of extreme pressure antiwear agent and 5-10 parts of structure improver.
The extreme pressure antiwear agent is one or more mixture selected from dialkyl dithiocarbamate, phosphate, borate and dialkyl dithiophosphate zinc.
Preferably, the extreme pressure antiwear agent is prepared from the following components in a mass ratio of (0.5-2): 1, or phosphate and borate ester with the mass ratio of 1: (1.5-2.5) zinc dialkyldithiophosphate and dialkyldithiocarbamate, or in a mass ratio of 1: (1.2-1.7): (0.3-0.7): (0.3-0.7) zinc dialkyldithiophosphates, dialkyldithiocarbamates, phosphate esters, and borate esters.
Preferably, the phosphate is one or a mixture of two of ashless dimethyl dithiophosphate and ammonium bis (2-ethylhexyl) phosphate. The borate is one or a mixture of two of nitrogen-containing borate and trimethyl borate.
In the system of the base oil and the structural modifier, the extreme pressure antiwear agent can endow the lubricating grease with better extreme pressure antiwear performance.
The thickening agent is prepared from 12-hydroxystearic acid, dibasic acid and lithium hydroxide.
Preferably, the dibasic acid is one or a mixture of two of azelaic acid and dodecanedioic acid.
In the thickener, the mass ratio of 12-hydroxystearic acid to dibasic acid is preferably (2-4): 1. the amount of lithium hydroxide used is calculated stoichiometrically.
The thickening agent can be well matched with a structure modifier and base oil to improve the mechanical stability and colloid stability of the lubricating grease.
Furthermore, the raw materials of the lubricating grease composition also comprise 0.5-3% by mass of an antioxidant, wherein the antioxidant is a mixture of 2, 6-di-tert-butyl-p-cresol and octyl butyl diphenylamine.
Preferably, the mass ratio of the 2, 6-di-tert-butyl-p-cresol to the octylbutyldiphenylamine is 1: (0.5-2).
The antioxidant can well play an antioxidant role in the base oil, the structure modifier and the thickener system used in the invention.
The raw materials of the lubricating grease composition also comprise 0.3-1.5% of antirust preservative by mass, and the antirust preservative is benzotriazole and zinc naphthenate.
Preferably, the mass ratio of the benzotriazole to the zinc naphthenate is 1: (1-2).
In the base oil, the structure modifier and the thickening agent system used in the invention, the antirust preservative can better ensure the antirust and radiation-proof performance of the lubricating grease.
The lubricating grease composition provided by the invention can be used as special lubricating grease for high-speed spinning spindles.
The invention also provides a preparation method of the lubricating grease composition, which comprises the following steps: saponifying a thickening agent raw material in part of base oil, adding the rest base oil and an antioxidant, cooling, performing high-pressure homogenization, adding an extreme pressure antiwear agent, a structure improver and an antirust preservative, performing high-pressure homogenization, and shearing.
The invention discovers that in the preparation process of the lubricating grease composition, the mixture of the base oil, the thickening agent and the antioxidant is subjected to high-pressure homogenizing dispersion treatment, and after other additives are added, the high-pressure homogenizing dispersion treatment and the shearing treatment are carried out, so that the mechanical stability and the colloid stability of the lubricating grease are improved, and the oil content of the lubricating grease is reduced.
Preferably, the high-pressure homogenizing pressure is 15-25 MPa. The shearing treatment is carried out by adopting a 0.7-0.9mm orifice plate and a 0.4-0.6mm orifice plate.
As a preferable scheme of the invention, the preparation method comprises the following steps: mixing 1/3 parts of base oil and 12-hydroxystearic acid, heating to 80-90 ℃, adding 35-45% of lithium hydroxide solution, and reacting for 55-65 min; adding dibasic acid at the temperature of 90-100 ℃, stirring for 40-50 minutes, and then beginning to dropwise add the rest lithium hydroxide solution at the temperature of 95-100 ℃; after the reaction is finished, stirring and heating to 140 ℃, and keeping the temperature for 30-60 min; heating to 200-180 ℃, adding base oil accounting for 1/3 of the total amount of the base oil, cooling to 150-180 ℃, adding all the antioxidant and the residual base oil, cooling to 100-120 ℃, dispersing by using a 18-22MPa high-pressure homogenizer, cooling to 80 ℃, adding the extreme pressure antiwear agent, the structure improver and the antirust preservative, stirring uniformly, dispersing by using a 18-22MPa high-pressure homogenizer, shearing by using a 0.8mm pore plate and a 0.5mm pore plate, filtering, degassing and canning to obtain the finished product.
The invention also provides application of the lubricating grease composition in lubrication of a high-speed spinning spindle.
The invention has the beneficial effects that: the lubricating grease composition provided by the invention has good adhesion performance and excellent anti-friction and anti-vibration performance, can effectively reduce friction resistance, reduce vibration and noise, save power consumption, and solve the problems of vibration, noise and energy consumption caused by high-speed operation of cotton spinning spindles. In addition, the lubricating grease composition provided by the invention has good mechanical stability and colloid stability, can ensure that a spinning spindle can stably and effectively run at a high rotating speed without loss, and solves the problem that cotton yarn is polluted by loss due to the fact that lubricating grease becomes thin and oil content is increased due to high-speed running of the spindle. The lubricating grease composition can meet the lubricating requirement of the spinning spindle under the working condition of high-rotating-speed operation at the speed of more than 20000 revolutions per minute, and can be used for lubricating the spinning spindle at the high rotating speed.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Unless otherwise specified, the technical means used in the following examples are conventional means well known to those skilled in the art, and the respective starting materials added are commercially conventional starting materials unless otherwise specified. Wherein the ethylene propylene rubber and the ethylene propylene diene rubber are purchased from China oil and gas group, and the mass fraction of ethylene in the product is 48.1-53.1%.
Example 1
This example provides a grease composition prepared from the following raw materials:
a thickening agent: 160kg of lithium hydroxide, wherein the mass ratio of the 12-hydroxystearic acid to the sebacic acid is 3: 1; lithium hydroxide: 34.8 Kg;
base oil: 1100kg (PAO synthetic oil: 40%, 150 BS: 60%, base oil kinematic viscosity at 40 ℃ 560 mm)2/s)；
Extreme pressure antiwear agent: 12.6kg of ashless dimethyl dithiophosphate and 12.6kg of nitrogen-containing boric acid ester;
antioxidant: 6.3kg of 2, 6-di-tert-butyl-p-cresol and 6.3kg of octyl butyl diphenylamine;
antirust and antiseptic: 3.78kg of benzotriazole and 6.3kg of zinc naphthenate;
structure improving agent: 25.2kg of ethylene propylene rubber.
This example also provides a preparation method of the grease composition, which specifically comprises the following steps:
mixing 1/3 parts of base oil and 12-hydroxystearic acid, heating to 83 ℃, adding 40% of lithium hydroxide solution, and reacting for 60 minutes; adding dibasic acid at the temperature of 98 ℃, stirring for 45 minutes, and then beginning to dropwise add the rest lithium hydroxide solution at the temperature of 97 ℃; after the reaction is finished, stirring and heating to 136 ℃, and keeping the temperature for 45 min; continuously heating to 208 ℃, adding base oil accounting for 1/3 of the total amount of the base oil for cooling, cooling to 165 ℃, adding all antioxidants and the rest base oil, cooling to 115 ℃, dispersing by using a 20MPa high-pressure homogenizer, cooling to below 80 ℃, adding an extreme pressure antiwear agent, a structure improver and an antirust preservative, uniformly stirring, dispersing by using the 20MPa high-pressure homogenizer, shearing by using a 0.8mm pore plate and a 0.5mm pore plate, filtering, degassing and canning to obtain the finished product.
Example 2
This example provides a grease composition prepared from the following raw materials:
a thickening agent: 160kg of a mixture of 12-hydroxystearic acid, sebacic acid and lithium hydroxide, wherein the mass ratio of the 12-hydroxystearic acid to the dodecanedioic acid is 3: 1; lithium hydroxide: 34.8 Kg;
base oil: 1100kg (PAO synthetic oil: 20%, 150 BS: 80%, base oil kinematic viscosity at 40 ℃ 370 mm)2/s)；
Extreme pressure antiwear agent: 12.6kg of zinc dialkyl dithiophosphate and 25.2kg of dialkyl dithiocarbamate;
antioxidant: 6.3kg of 2, 6-di-tert-butyl-p-cresol and 6.3kg of octyl butyl diphenylamine;
antirust and antiseptic: 6.3kg of benzotriazole and 6.3kg of zinc naphthenate;
structure improving agent: 25.2kg of ethylene propylene diene monomer.
This example also provides a preparation method of the grease composition, which specifically comprises the following steps:
mixing 1/3 parts of base oil and 12-hydroxystearic acid, heating to 85 ℃, adding 40% of lithium hydroxide solution, and reacting for 60 minutes; adding dibasic acid at 97 deg.c, stirring for 45min and dropping residual lithium hydroxide solution at 98 deg.c; after the reaction is finished, stirring and heating to 135 ℃, and keeping the temperature for 45 min; continuously heating to 210 ℃, adding base oil accounting for 1/3 of the total amount of the base oil for cooling, cooling to 160 ℃, adding all antioxidants and the rest base oil, cooling to 112 ℃, dispersing by using a 20MPa high-pressure homogenizer, cooling to below 80 ℃, adding an extreme pressure antiwear agent, a structure improver and an antirust preservative, uniformly stirring, dispersing by using the 20MPa high-pressure homogenizer, shearing by using a 0.8mm pore plate and a 0.5mm pore plate, filtering, degassing and canning to obtain the finished product.
Example 3
This example provides a grease composition prepared from the following raw materials:
a thickening agent: 160kg of a mixture of 12-hydroxystearic acid, sebacic acid and lithium hydroxide, wherein the mass ratio of the 12-hydroxystearic acid to the dodecanedioic acid is 3: 1; lithium hydroxide: 34.8 Kg;
base oil: 1100kg (PAO synthetic oil: 20%, 150 BS: 80%, base oil kinematic viscosity at 40 ℃ 420 mm)2/s)；
Extreme pressure antiwear agent: 12.6kg of zinc dialkyldithiophosphate, 18.9kg of dialkyldithiocarbamate, 6.3kg of ammonium di (2-ethylhexyl) phosphate and 6.3kg of trimethyl borate;
antioxidant: 6.3kg of 2, 6-di-tert-butyl-p-cresol and 6.3kg of octyl butyl diphenylamine;
antirust and antiseptic: 6.3kg of benzotriazole and 6.3kg of zinc naphthenate;
structure improving agent: 12.6kg of ethylene propylene rubber and 12.6kg of ethylene propylene diene monomer.
This example also provides a method for preparing the grease composition described above, which is the same as the method for preparing example 1.
Comparative example 1
The present comparative example provides a grease composition prepared as follows:
a thickening agent: 160kg of lithium hydroxide, wherein the mass ratio of the 12-hydroxystearic acid to the sebacic acid is 3: 1; lithium hydroxide: 34.8 Kg;
base oil: 1100kg (PAO synthetic oil: 40%, 150 BS: 60%, base oil kinematic viscosity at 40 ℃ 560 mm)2/s)；
Extreme pressure antiwear agent: 12.6kg of ashless dimethyl dithiophosphate and 12.6kg of nitrogen-containing boric acid ester;
antioxidant: 6.3kg of 2, 6-di-tert-butyl-p-cresol and 6.3kg of octyl butyl diphenylamine;
antirust and antiseptic: 3.78kg of benzotriazole and 6.3kg of zinc naphthenate;
structure improving agent: 25.2kg of ethylene propylene rubber.
The present comparative example also provides a method for preparing the grease composition described above, specifically as follows:
mixing 1/3 parts of base oil and 12-hydroxystearic acid, heating to 83 ℃, adding 40% of lithium hydroxide solution, and reacting for 60 minutes; adding dibasic acid at the temperature of 98 ℃, stirring for 45 minutes, and then beginning to dropwise add the rest lithium hydroxide solution at the temperature of 97 ℃; after the reaction is finished, stirring and heating to 136 ℃, and keeping the temperature for 45 min; and continuously heating to 208 ℃, adding base oil accounting for 1/3 of the total amount of the base oil for cooling, cooling to 165 ℃, adding all the antioxidants and the residual base oil, cooling to below 80 ℃, adding the extreme pressure antiwear agent, the structure improver and the antirust preservative, uniformly stirring, filtering, degassing and canning to obtain the finished product.
Comparative example 2
The present comparative example provides a grease composition prepared as follows:
a thickening agent: 160kg of a mixture of 12-hydroxystearic acid, sebacic acid and lithium hydroxide, wherein the mass ratio of the 12-hydroxystearic acid to the dodecanedioic acid is 3: 1; lithium hydroxide: 34.8 Kg;
base oil: 1100kg (PAO synthetic oil: 20%, 150 BS: 80%, base oil kinematic viscosity at 40 ℃ 370 mm)2/s)；
Extreme pressure antiwear agent: 12.6kg of zinc dialkyl dithiophosphate and 25.2kg of dialkyl dithiocarbamate;
antioxidant: 6.3kg of 2, 6-di-tert-butyl-p-cresol and 6.3kg of octyl butyl diphenylamine;
antirust and antiseptic: 6.3kg of benzotriazole and 6.3kg of zinc naphthenate;
this comparative example also provides a method for preparing the grease composition described above, which differs from the preparation method of example 2 only in that: no structural modifier was added.
Comparative example 3
The present comparative example provides a grease composition prepared as follows:
a thickening agent: 160kg of a mixture of 12-hydroxystearic acid, sebacic acid and lithium hydroxide, wherein the mass ratio of the 12-hydroxystearic acid to the dodecanedioic acid is 3: 1; lithium hydroxide: 34.8 Kg;
base oil: 1100kg (mineral oil 100%, base oil kinematic viscosity at 40 ℃ 120 mm)2/s)；
Extreme pressure antiwear agent: 12.6kg of zinc dialkyldithiophosphate, 18.9kg of dialkyldithiocarbamate, 6.3kg of ammonium di (2-ethylhexyl) phosphate and 6.3kg of trimethyl borate;
antioxidant: 6.3kg of 2, 6-di-tert-butyl-p-cresol and 6.3kg of octyl butyl diphenylamine;
antirust and antiseptic: 6.3kg of benzotriazole and 6.3kg of zinc naphthenate;
structure improving agent: 12.6kg of ethylene propylene rubber and 12.6kg of ethylene propylene diene monomer.
This comparative example also provides the same preparation method as example 3 for the grease composition described above.
Examples of the experiments
The performance of the greases obtained in examples 1 to 3 and comparative examples 1 to 3 was tested, and the test results are shown in table 1.
Table 1 grease performance test results
Figure BDA0003213461460000101
The above results show that the grease compositions prepared in the embodiments 1 to 3 of the present invention all exhibit excellent mechanical stability, colloid stability and wear and vibration resistance, and completely meet the working condition requirements of high-speed spindles on grease. The lubricating grease composition disclosed by the invention can provide more reliable and comprehensive protection for using equipment, and has a good application prospect.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (10)

1. A lubricating grease composition is characterized by being prepared from the following raw materials: thickening agent, base oil, extreme pressure antiwear agent and structure improver,
the structure improver is one or a mixture of two of ethylene propylene rubber and ethylene propylene diene monomer,
the kinematic viscosity at 40 ℃ of the base oil is 200-600mm2/s，
The mass ratio of the structure improver to the base oil is (0.01-0.05): 1.
2. a grease composition according to claim 1, wherein the base oil is a mixture of, by mass, 1: the PAO synthetic oil of (1-5) and 150BS base oil.
3. The grease composition according to claim 1, wherein when the structure improver is ethylene propylene rubber and ethylene propylene diene rubber, the mass ratio of the ethylene propylene rubber to the ethylene propylene diene rubber is (0.5-2): 1.
4. a lubricating grease composition according to any one of claims 1 to 3, characterized in that the raw materials thereof comprise the following components in parts by weight: 5-10 parts of thickening agent, 60-80 parts of base oil, 0.5-5 parts of extreme pressure antiwear agent and 5-10 parts of structure improver.
5. The grease composition of claim 4, wherein the extreme pressure antiwear agent is a mixture of one or more selected from the group consisting of dialkyl dithiocarbamates, phosphate esters, borate esters, and zinc dialkyl dithiophosphates;
preferably, the extreme pressure antiwear agent is prepared from the following components in a mass ratio of (0.5-2): 1, or phosphate and borate ester with the mass ratio of 1: (1.5-2.5) zinc dialkyldithiophosphate and dialkyldithiocarbamate, or in a mass ratio of 1: (1.2-1.7): (0.3-0.7): (0.3-0.7) zinc dialkyldithiophosphates, dialkyldithiocarbamates, phosphate esters, and borate esters.
6. A grease composition according to claim 4 or 5, characterized in that the thickener is prepared from 12-hydroxystearic acid, a dibasic acid and lithium hydroxide;
preferably, the dibasic acid is one or a mixture of two selected from azelaic acid and dodecanedioic acid.
7. The lubricating grease composition according to any one of claims 1 to 6, characterized in that the raw materials further comprise 0.5 to 3 mass percent of an antioxidant, wherein the antioxidant is a mixture of 2, 6-di-tert-butyl-p-cresol and octyl butyl diphenylamine;
preferably, the mass ratio of the 2, 6-di-tert-butyl-p-cresol to the octylbutyldiphenylamine is 1: (0.5-2).
8. The lubricating grease composition according to any one of claims 1 to 7, characterized in that the raw materials further comprise 0.3 to 1.5 mass percent of an anti-rust preservative, wherein the anti-rust preservative is benzotriazole and zinc naphthenate;
preferably, the mass ratio of the benzotriazole to the zinc naphthenate is 1: (1-2).
9. A method for preparing a grease composition according to any one of claims 1 to 8, comprising the steps of: saponifying a thickening agent raw material in part of base oil, adding the rest base oil and an antioxidant, cooling, performing high-pressure homogenization, adding an extreme pressure antiwear agent, a structure improver and an antirust preservative, performing high-pressure homogenization, and shearing;
preferably, the high-pressure homogenizing pressure is 15-25MPa, and/or the shearing treatment is performed by using a 0.7-0.9mm orifice plate and a 0.4-0.6mm orifice plate.
10. Use of a grease composition according to any one of claims 1 to 8 for lubrication of a high speed spinning spindle.
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