CN111040830B - Lubricating grease and preparation method thereof - Google Patents

Lubricating grease and preparation method thereof Download PDF

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Publication number
CN111040830B
CN111040830B CN201811182969.XA CN201811182969A CN111040830B CN 111040830 B CN111040830 B CN 111040830B CN 201811182969 A CN201811182969 A CN 201811182969A CN 111040830 B CN111040830 B CN 111040830B
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oil
parts
lubricating grease
grease
base oil
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CN111040830A (en
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叶晶
黄永恒
李旻彦
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OFilm Image Technology Guangzhou Co Ltd
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OFilm Image Technology Guangzhou 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
    • C10M169/04—Mixtures of base-materials and additives
    • C10M169/048—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution, non-macromolecular and macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08—Inorganic acids or salts thereof
    • C10M2201/084—Inorganic acids or salts thereof 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
    • 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
    • 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
    • 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
    • C10M2207/40—Fatty vegetable or animal oils
    • C10M2207/401—Fatty vegetable or animal oils 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
    • C10M2207/40—Fatty vegetable or animal oils
    • C10M2207/402—Castor oils
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2213/02—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions obtained from monomers containing carbon, hydrogen and halogen 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
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/30—Heterocyclic compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
    • 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
    • C10M2219/068—Thiocarbamate metal salts
    • 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
    • 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

Abstract

The invention relates to lubricating grease and a preparation method thereof. The lubricating grease is prepared from 77-92 parts by mass of base oil, 10.3-17.6 parts by mass of thickening agent and 5-8 parts by mass of polymetallic oxygen cluster compound, wherein the base oil comprises bio-oil and synthetic oil, and the polymetallic oxygen cluster compound has a nucleophilic group and an electrophilic group. The lubricating grease has better adsorbability to micron-sized steel scraps through the synergistic effect of the base oil and the multi-metal oxygen cluster compound.

Description

Lubricating grease and preparation method thereof
Technical Field
The invention relates to the technical field of lubrication, in particular to lubricating grease and a preparation method thereof.
Background
The used mechanical equipment of camera module processing can produce the tiny iron and steel piece of micron order (SUS) because of long-term the use, the tiny iron and steel piece of micron order can carry on the in-process at the camera spare part and get into inside the camera module, and the optical imaging to the module produces the interference, has directly influenced the imaging quality of module.
In order to avoid the generation of steel scrap in mechanical equipment, the equipment is generally regularly maintained and surface treatments such as lubrication are applied to mechanical parts. However, the current grease has poor adsorption to micron-sized steel chips, which affects the production yield and efficiency of the product.
Disclosure of Invention
Accordingly, there is a need for a grease that has good adsorption to steel scrap on the micron scale.
In addition, a preparation method of the lubricating grease is also provided.
The lubricating grease is prepared from the following raw materials in parts by mass:
77-92 parts of base oil;
10.3 to 17.6 portions of thickening agent;
5-8 parts of a multi-metal oxygen cluster compound;
wherein the base oil comprises bio-oil and synthetic oil, and the polyoxometalate compound has a nucleophilic group and an electrophilic group.
The base oil of the lubricant is compounded by adopting the biological oil and the synthetic oil, so that the base oil has good adhesiveness and is not easy to run off, and can be firmly adhered to the mechanical lubrication surface to form a grease ring with a sealing effect, and steel scraps generated by the friction of mechanical parts are difficult to separate after being adsorbed, thereby fundamentally improving the problem of the steel scraps generated by mechanical equipment; the thickening agent is dispersed in the base oil to form a structural framework, and the base oil is adsorbed and fixed in the structural framework, so that the semi-solid lubricating grease with plasticity is formed; meanwhile, the polymetallic oxygen cluster compound dispersed in the base oil has a nucleophilic group and an electrophilic group, and the molecular chain end of the polymetallic oxygen cluster compound has strong electrostatic attraction, so that micron-sized fine steel chips can be adsorbed. The lubricating grease has good adsorbability on micron-sized steel scraps through the synergistic effect of the base oil, the thickening agent and the multi-metal oxygen cluster compound.
In one embodiment, the multimetal oxygen cluster compound has the formula [ Cu ]I(2,2'-bipy)2]{[CuI(2,2'-bipy)2]2][PW12O40]}. The polymetallic oxygen cluster compound can make the adsorption of the lubricating grease better.
In one embodiment, the thickener is selected from at least one of a sodium-based thickener, an aluminum-based thickener, and a lithium-based thickener. The thickening agent is dispersed in the base oil to form a structural framework, and the base oil is adsorbed and fixed in the structural framework, so that the semi-solid lubricating grease with plasticity is formed.
In one embodiment, the sodium-based thickener is selected from at least one of sodium sebacate and sodium salicylate; the aluminum-based thickening agent is alum; the lithium-based thickener is at least one selected from lithium 12-hydroxystearate and lithium borate.
In one embodiment, the bio-oil is selected from at least one of an animal oil and a vegetable oil; and/or the synthetic oil is selected from at least one of neopentyl glycol ester, trimethylolpropane ester and pentaerythritol ester. The animal oil and/or vegetable oil and the synthetic oil are compounded, so that the obtained base oil has good adhesion and is difficult to run off, the base oil can be firmly adhered to the mechanical lubrication surface to form a grease ring with a sealing effect, steel scraps generated by the friction of mechanical parts are adsorbed and difficult to separate, and the problem of the steel scraps generated by mechanical equipment is fundamentally solved.
In one embodiment, the bio-oil is selected from at least one of animal oil and vegetable oil selected from at least one of castor oil, sunflower oil and soybean oil; the animal oil is at least one selected from beef tallow, lard and mutton fat.
In one embodiment, the raw materials for preparing the grease also comprise 0.4-0.7 part of extreme pressure antiwear agent, and the extreme pressure antiwear agent is selected from at least one of sulfurized whale oil, sulfurized olefin, triethyl phosphate, dibutyl phosphite and chlorinated paraffin, so that the grease has better extreme pressure antiwear capacity.
In one embodiment, the raw materials for preparing the lubricating grease further comprise 1-2 parts of antioxidant, and the antioxidant is selected from at least one of dialkyl dithiocarbamate, diphenylamine and N-N-butyl-p-aminophenol, so that the lubricating grease has better antioxidant capacity.
In one embodiment, the raw material for preparing the grease also comprises 3.5-6 parts of an antirust agent, and the antirust agent is selected from at least one of barium petroleum sulfonate, calcium petroleum sulfonate, sorbitol monooleate and sodium nitrite, so that the grease has better antirust capacity.
In one embodiment, the raw materials for preparing the lubricating grease further comprise 0.2-0.3 part of a preservative selected from at least one of benzotriazole and benzothiazole, so that the lubricating grease has better durability.
A preparation method of lubricating grease comprises the following steps:
preparing raw materials: preparing 77-92 parts of base oil, 10.3-17.6 parts of thickening agent and 5-8 parts of multi-metal oxide cluster compound according to the mass parts;
mixing raw materials: mixing the base oil, the thickener and the multi-metal oxide cluster compound at 70-80 ℃ to obtain a premix;
saponification dehydration cooling: under the conditions of 0.5MPa to 0.6MPa and 170 ℃ to 180 ℃, the pre-mixture is firstly saponified for 70min to 80min, then dehydrated for 20min to 30min under constant pressure, and then cooled to 75 ℃ to 80 ℃ to obtain the lubricating grease.
The preparation method of the lubricating grease is simple in process and suitable for industrial production.
In one embodiment, after the saponification dehydration cooling step, at least one of the following steps is further included:
and (3) extreme pressure antiwear treatment: firstly, adding an extreme pressure antiwear agent at 70-80 ℃, and then stirring at the rotating speed of 70-80 r/min for 60-70 min;
and (3) antioxidant treatment: firstly, adding an antioxidant at 70-80 ℃, and then stirring at a rotating speed of 70-80 r/min for 60-70 min;
performing rust prevention treatment: adding an antirust agent at 70-80 ℃, and then stirring at a rotating speed of 70-80 r/min for 60-70 min;
and (3) antiseptic treatment: firstly, adding the preservative at 70-80 ℃, and then stirring at the rotating speed of 70-80 r/min for 60-70 min.
The preparation method and the process of the lubricating grease can be used for users to flexibly select the combination of process steps to prepare the lubricating grease meeting the actual requirements of different mechanical equipment.
Detailed Description
The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The lubricating grease of an embodiment is prepared from the following raw materials in parts by mass:
77-92 parts of base oil;
10.3 to 17.6 portions of thickening agent;
5-8 parts of a multi-metal oxygen cluster compound.
Wherein the base oil comprises biological oil and synthetic oil. The biological oil and the synthetic oil are compounded, so that the obtained base oil has good adhesion and is not easy to run off, the base oil can be firmly adhered to the mechanical lubrication surface to form a grease ring with a sealing effect, and steel scraps (SUS) generated by the friction of mechanical parts are difficult to separate after being adsorbed, so that the problem of the steel scraps generated by mechanical equipment is fundamentally solved, the cleanliness of the equipment in the production process is improved, and an electronic product can not be influenced by the steel scraps in the assembling process. Further, the biological oil accounts for 60-70 parts by weight; the synthetic oil accounts for 17-22 parts by mass.
Further, the bio-oil includes vegetable oil and animal oil. Further, the vegetable oil is selected from at least one of castor oil, sunflower seed oil and soybean oil; the animal oil is at least one selected from adeps medulla bovis Seu Bubali, adeps Sus Domestica and adeps Caprae Seu Ovis. Specifically, the vegetable oil is 30-35 parts by weight; the animal oil accounts for 30-35 parts by weight. Wherein, the castor oil, the sunflower seed oil and the soybean oil are all liquid, the beef tallow is liquid or solid, the lard is liquid or solid, and the mutton fat is liquid or solid.
Further, the synthetic oil is selected from at least one of neopentyl glycol ester, trimethylolpropane ester and pentaerythritol ester. Wherein, neopentyl glycol ester is liquid or solid, trimethylolpropane ester is liquid or solid, and pentaerythritol ester is liquid or solid.
Specifically, the base oil is a mixture of castor oil, tallow, neopentyl glycol ester and pentaerythritol ester. Further, the mass portion of the castor oil is 30-35; the mass portion of the beef tallow is 30-35; the weight portion of neopentyl glycol ester is 9-12; the mass portion of the pentaerythritol ester is 8 to 10. Furthermore, the mass ratio of the castor oil to the tallow, the neopentyl glycol ester and the pentaerythritol ester is 3:3:1: 1.
Wherein the thickener is at least one of sodium-based thickener, aluminum-based thickener and lithium-based thickener. The thickening agent is dispersed in the base oil to form a structural framework, and the base oil is adsorbed and fixed in the structural framework, so that the semi-solid lubricating grease with plasticity is formed. Further, the sodium-based thickening agent is selected from at least one of sodium sebacate and sodium salicylate; the aluminum-based thickening agent is alum; the lithium-based thickener is at least one selected from lithium 12-hydroxystearate and lithium borate. The molecular chain of the thickening agent is appropriate in length, has more excellent van der Waals force and capillary action, and can adsorb the base oil more stably to form grease. Wherein the sodium-based thickener, the aluminum-based thickener and the lithium-based thickener are all solids.
The multimetal oxygen cluster compound has a nucleophilic group and an electrophilic group. The ionic force of the chain end of the thickening agent compounded by the multi-metal oxygen cluster compound and the thickening agent is stronger, and stable reticular structure fiber can be formed. The polymetallic oxygen cluster compound dispersed in the base oil has stronger electrostatic attraction at the molecular chain end, can adsorb micron-sized fine steel chips, and has better adsorbability and usability as a whole. Specifically, the molecular formula of the multimetal oxygen cluster compound is [ Cu ]I(2,2'-bipy)2]{[CuI(2,2'-bipy)2]2][PW12O40]}. Wherein the multi-metal oxygen cluster compound is solid.
The lubricating grease further comprises 0.4-0.7 part of extreme pressure antiwear agent by weight, so that the lubricating grease has good extreme pressure antiwear capacity. Further, the extreme pressure antiwear agent is selected from at least one of sulfurized whale oil, sulfurized olefin, triethyl phosphate, dibutyl phosphite and chlorinated paraffin. Specifically, the extreme pressure antiwear agent is a mixture of sulfurized whale oil, triethyl phosphate and chlorinated paraffin. More specifically, the mass ratio of the sulfurized whale oil to the triethyl phosphate and the chlorinated paraffin is 3:2:2, so that better load resistance and abrasion resistance are provided, the generation of steel fines in the production process of electronic products by mechanical equipment is reduced, the problem of the steel fines generated by the equipment is improved from the source, and the electronic products are not influenced by the steel fines in the assembling process. Wherein the sulfurized whale oil, sulfurized olefin, triethyl phosphate, dibutyl phosphite and chlorinated paraffin are all liquid.
The lubricating grease further comprises 1-2 parts of antioxidant by mass, so that the lubricating grease has good antioxidant capacity. Further, the antioxidant is selected from at least one of dialkyldithiocarbamate, diphenylamine and N-N-butyl-p-aminophenol. Still further, the antioxidant is a dialkyldithiocarbamate. Wherein the dialkyl dithiocarbamate, diphenylamine and N-N-butyl-p-aminophenol are all solid.
The grease also comprises 3.5 to 6 parts of antirust agent by weight, so that the grease has better antirust capacity. Further, the rust inhibitor is at least one selected from barium petroleum sulfonate, calcium petroleum sulfonate, sorbitol monooleate and sodium nitrite. Specifically, the rust inhibitor is a mixture of barium petroleum sulfonate and sorbitol monooleate. More specifically, the mass ratio of barium petroleum sulfonate to sorbitol monooleate was 6: 1. Wherein, the barium petroleum sulfonate is liquid or semisolid, the calcium petroleum sulfonate is liquid or semisolid, the sorbitol monooleate is liquid or semisolid, and the sodium nitrite is solid.
The lubricating grease further comprises 0.2-0.3 part of preservative by mass so as to enable the lubricating grease to have better durability. Further, the preservative is selected from at least one of benzotriazole and benzothiazole. Further, the preservative is benzotriazole. Wherein, the benzotriazole is solid, and the benzothiazole is liquid.
The grease has at least the following advantages:
1) the base oil of the lubricant is compounded by adopting the biological oil and the synthetic oil, so that the base oil has good adhesiveness and is not easy to run off, and can be firmly adhered to the mechanical lubrication surface to form a grease ring with a sealing effect, and steel scraps generated by the friction of mechanical parts are difficult to separate after being adsorbed, thereby fundamentally improving the problem of the steel scraps generated by mechanical equipment; meanwhile, the polymetallic oxygen cluster compound dispersed in the base oil has a nucleophilic group and an electrophilic group, and the molecular chain end of the polymetallic oxygen cluster compound has strong electrostatic attraction, so that micron-sized fine steel chips can be adsorbed. The lubricating grease has better adsorption to micron-sized steel scraps through the synergistic action of the base oil and the multi-metal oxygen cluster compound.
2) The molecular chain length of the thickening agent is appropriate, the thickening agent has more excellent Van der Waals force and capillary action, and can adsorb base oil more stably to form grease, and meanwhile, the thickening agent and the multi-metal oxygen cluster compound are compounded according to a certain proportion, so that the ionic force at the chain end of the thickening agent is stronger, more stable network structure fibers are formed, and the lubricating grease is more stable.
3) The base oil of the lubricating oil is prepared by compounding animal oil and/or vegetable oil with synthetic oil, so that the obtained base oil has good adhesion and is difficult to run off, can be firmly adhered to the surface of mechanical lubrication to form a grease ring with a sealing effect, adsorbs steel scrap (SUS) generated by friction of mechanical parts and is difficult to separate, the problem of the steel scrap generated by mechanical equipment is fundamentally solved, the cleanliness of the equipment in the production process is improved, and an electronic product is not influenced by steel scrap in the assembling process.
4) The extreme pressure antiwear agent in the lubricating grease is a mixture of vulcanized whale oil, triethyl phosphate and chlorinated paraffin, and the mass ratio of the vulcanized whale oil to the triethyl phosphate to the chlorinated paraffin is 3:2:2, so that better anti-load capacity and anti-wear capacity can be provided, the generation of steel fines in the production process of electronic products by mechanical equipment is reduced, the problem of the steel fines generated by the equipment is improved from the source, and the electronic products are not influenced by the steel fines in the assembly process.
A method for producing a grease of an embodiment is one of the above-described greases, and includes the steps of:
and mixing the base oil, the thickening agent and the multi-metal oxygen cluster compound at the temperature of 70-80 ℃ to obtain the lubricating grease.
Wherein the base oil comprises 77-92 parts by weight of biological oil and synthetic oil. Further, the mass portion of the biological oil is 60 to 70; the synthetic oil accounts for 17-22 parts by mass.
Further, the bio-oil includes vegetable oil and animal oil. Further, the vegetable oil is selected from at least one of castor oil, sunflower seed oil and soybean oil; the animal oil is at least one selected from adeps medulla bovis Seu Bubali, adeps Sus Domestica and adeps Caprae Seu Ovis. Specifically, the vegetable oil accounts for 30-35 parts by weight; the animal oil accounts for 30-35 parts by weight. Wherein, the castor oil, the sunflower seed oil and the soybean oil are all liquid, the beef tallow is liquid or solid, the lard is liquid or solid, and the mutton fat is liquid or solid.
Further, the synthetic oil is selected from at least one of neopentylene glycol ester and pentaerythritol ester. Wherein, neopentyl glycol ester is liquid or solid, trimethylolpropane ester is liquid or solid, and pentaerythritol ester is liquid or solid.
Specifically, the base oil is a mixture of castor oil, tallow, neopentyl glycol ester and pentaerythritol ester. Further, the mass portion of the castor oil is 30-35; the mass portion of the beef tallow is 30-35; the weight portion of the neopentyl glycol ester is 9 to 12 portions; the mass portion of the pentaerythritol ester is 8 to 10. Furthermore, the mass ratio of the castor oil to the tallow, the neopentyl glycol ester and the pentaerythritol ester is 3:3:1: 1.
Wherein the mass portion of the thickening agent is 10.3-17.6. Further, the thickener is at least one selected from a sodium-based thickener, an aluminum-based thickener, and a lithium-based thickener. Further, the sodium-based thickener is at least one selected from sodium sebacate and sodium salicylate; the aluminum-based thickening agent is alum; the lithium-based thickener is at least one selected from lithium 12-hydroxystearate and lithium borate. The molecular chain of the thickening agent is appropriate in length, has more excellent van der Waals force and capillary action, and can adsorb base oil more stably to form grease. Wherein the sodium-based thickener, the aluminum-based thickener and the lithium-based thickener are all solids.
Wherein the multimetal oxygen cluster compound has a nucleophilic group and an electrophilic group. Further, the mass part of the multi-metal oxygen cluster compound is 5-8 parts. Specifically, the molecular formula of the multimetal oxygen cluster compound is [ Cu ]I(2,2'-bipy)2]{[CuI(2,2'-bipy)2]2][PW12O40]}. Wherein the multi-metal oxygen cluster compound is solid.
Further, the step of mixing the base oil, the thickening agent and the multi-metal oxide cluster compound specifically comprises the following steps: the base oil, the thickening agent and the multi-metal oxygen cluster compound are stirred for 30-40 min at the rotating speed of 50-60 r/min.
When the thickener is a sodium-based thickener, the raw materials of the sodium-based thickener include an organic acid and sodium hydroxide. Further, the organic acid is at least one selected from sebacic acid and salicylic acid. At the moment, the mixing steps of the base oil, the thickening agent and the multi-metal oxygen cluster compound are as follows:
mixing base oil, organic acid and a polymetallic oxygen cluster compound at 70-80 ℃ to obtain a premix;
and (2) carrying out saponification reaction on the premix and a sodium hydroxide solution under the conditions of 0.5-0.6 MPa and 170-180 ℃ to obtain the lubricating grease, wherein the saponification reaction time is 70-80 min. Wherein the solvent in the sodium hydroxide solution is selected from one of water for soap, deionized water and distilled water. Specifically, the sodium hydroxide solution is 2 to 3.5 parts by weight. More specifically, the mass part of the sodium hydroxide is 1-2 parts; the mass portion of the solvent in the sodium hydroxide solution is 1-1.5.
Further, the step of saponifying the premix with sodium hydroxide solution may be followed by a step of dehydrating and cooling. Specifically, the dehydration step is: dehydrating for 20min to 30min at constant pressure, and then dehydrating for 10min to 15min while exhausting air; the cooling steps are specifically as follows: slowly cooling to 75-80 ℃.
The lubricating grease is prepared by the steps of mixing base oil, a thickening agent and a multi-metal oxygen cluster compound, adding an extreme pressure antiwear agent at 70-80 ℃, and stirring at a rotating speed of 70-80 r/min for 60-70 min to obtain the lubricating grease, wherein the weight part of the extreme pressure antiwear agent is 0.4-0.7 part. Further, the extreme pressure antiwear agent is selected from at least one of sulfurized whale oil, sulfurized olefin, triethyl phosphate, dibutyl phosphite and chlorinated paraffin. Specifically, the extreme pressure antiwear agent is a mixture of sulfurized whale oil, triethyl phosphate and chlorinated paraffin. More specifically, the mass ratio of the sulfurized whale oil to the triethyl phosphate and the chlorinated paraffin is 3:2:2, so that better load resistance and abrasion resistance are provided, the generation of steel fines in the production process of electronic products by mechanical equipment is reduced, the problem of the steel fines generated by the equipment is improved from the source, and the electronic products are not influenced by the steel fines in the assembling process. Wherein the sulfurized whale oil, sulfurized olefin, triethyl phosphate, dibutyl phosphite and chlorinated paraffin are all liquid.
The lubricating grease is prepared by the steps of mixing base oil, a thickening agent and a multi-metal oxygen cluster compound, adding an antioxidant at 70-80 ℃, and stirring at a rotating speed of 70-80 r/min for 60-70 min to obtain the lubricating grease, wherein the mass part of the antioxidant is 1-2 parts. Further, the antioxidant is selected from at least one of dialkyldithiocarbamate, diphenylamine and N-N-butyl-p-aminophenol. Still further, the antioxidant is a dialkyldithiocarbamate. Wherein the dialkyl dithiocarbamate, diphenylamine and N-N-butyl-p-aminophenol are all solid.
The lubricating grease is prepared by the steps of mixing base oil, a thickening agent and a multi-metal oxide cluster compound, adding an antirust agent at 70-80 ℃, and stirring at a rotating speed of 70-80 r/min for 60-70 min to obtain the lubricating grease, wherein the antirust agent is 3.5-6 parts by weight. Further, the rust inhibitor is at least one selected from barium petroleum sulfonate, calcium petroleum sulfonate, sorbitol monooleate, and sodium nitrite. Specifically, the rust inhibitor is a mixture of barium petroleum sulfonate and sorbitol monooleate. More specifically, the mass ratio of barium petroleum sulfonate to sorbitol monooleate was 6: 1. Wherein, the barium petroleum sulfonate is liquid or semisolid, the calcium petroleum sulfonate is liquid or semisolid, the sorbitol monooleate is liquid or semisolid, and the sodium nitrite is solid.
The lubricating grease is prepared by the steps of mixing base oil, a thickening agent and a multi-metal oxygen cluster compound, adding a preservative at 70-80 ℃, and stirring at a rotating speed of 70-80 r/min for 60-70 min to obtain the lubricating grease, wherein the preservative is 0.2-0.3 part by mass. Further, the preservative is selected from at least one of benzotriazole and benzothiazole. Further, the preservative is benzotriazole. Wherein, the benzotriazole is solid, and the benzothiazole is liquid.
The preparation method of the lubricating grease is simple in process and suitable for industrial production.
The lubricating grease and the lubricating grease prepared by the preparation method of the lubricating grease are applied to mechanical equipment. For example, in mechanical equipment for manufacturing camera modules.
The following are specific examples:
example 1
The grease of this example was prepared as follows:
(1) according to the mass parts, 30 parts of castor oil, 30 parts of beef tallow, 9 parts of neopentyl glycol ester and 8 parts of pentaerythritol ester are uniformly mixed and added into a reaction kettle, 5 parts of polyoxometalate compound, 4 parts of sebacic acid, 2 parts of salicylic acid, 0.3 part of alum and 3 parts of lithium 12-hydroxystearate are sequentially added, then the reaction kettle is heated to 70 ℃, and is stirred for 30min at the rotating speed of 50r/min, so that a premix is obtained.
(2) Dissolving 1 part of sodium hydroxide in 1 part of soap water by mass to obtain an alkali solution; adding the alkali solution and the premix into a reaction kettle, uniformly mixing, heating and pressurizing the reaction kettle to 170 ℃ and 0.5Mpa, saponifying at constant pressure for 70min, dehydrating at constant pressure for 20min, dehydrating while exhausting air for 10min, and slowly cooling to 75 ℃ to obtain a mixture.
(3) According to the mass parts, 1 part of dialkyl dithiocarbamate, 0.2 part of sulfurized whale oil, 0.1 part of triethyl phosphate, 0.1 part of chlorinated paraffin, 3 parts of barium petroleum sulfonate, 0.5 part of sorbitol monooleate and 0.2 part of benzotriazole are sequentially added into the mixture at the temperature of 70 ℃, and the mixture is stirred for 60min at the rotating speed of 70r/min to obtain the lubricating grease.
Example 2
The grease of this example was prepared as follows:
(1) according to the mass parts, 32 parts of castor oil, 32 parts of beef tallow, 10 parts of neopentyl glycol ester and 9 parts of pentaerythritol ester are uniformly mixed and added into a reaction kettle, 6 parts of polyoxometalate compound, 5 parts of sebacic acid, 3 parts of salicylic acid, 0.5 part of alum and 4 parts of lithium 12-hydroxystearate are sequentially added, then the reaction kettle is heated to 75 ℃, and the mixture is stirred for 35min at the rotating speed of 55r/min, so that a premix is obtained.
(2) Dissolving 1 part of sodium hydroxide in 1 part of soap water by mass to obtain an alkali solution; adding alkali solution into a reaction kettle, mixing with the premix uniformly, heating and pressurizing the reaction kettle to 175 ℃ and 0.6Mpa, saponifying at constant pressure for 75min, dehydrating at constant pressure for 25min, dehydrating while exhausting air for 12min, and cooling to 78 ℃ to obtain a mixture.
(3) According to the mass parts, 1 part of dialkyl dithiocarbamate, 0.2 part of sulfurized whale oil, 0.2 part of triethyl phosphate, 0.2 part of chlorinated paraffin, 3 parts of barium petroleum sulfonate, 0.5 part of sorbitol monooleate and 0.3 part of benzotriazole are sequentially added into the mixture at the temperature of 75 ℃, and the mixture is stirred for 65min at the rotating speed of 75r/min to obtain the lubricating grease.
Example 3
The grease of this example was prepared as follows:
(1) according to the mass parts, 35 parts of castor oil, 35 parts of beef tallow, 12 parts of neopentyl glycol ester and 10 parts of pentaerythritol ester are uniformly mixed and added into a reaction kettle, 8 parts of polyoxometalate compound, 6 parts of sebacic acid, 4 parts of salicylic acid, 0.6 part of alum and 5 parts of lithium 12-hydroxystearate are sequentially added, then the reaction kettle is heated to 80 ℃, and the mixture is stirred for 40min at the rotating speed of 60r/min, so that the premix is obtained.
(2) Dissolving 2 parts by weight of sodium hydroxide in 1.5 parts by weight of soap water to obtain an alkali solution; adding the alkali solution into a reaction kettle, uniformly mixing with the premix, heating and pressurizing the reaction kettle to 180 ℃ and 0.6Mpa, saponifying at constant pressure for 80min, dehydrating at constant pressure for 30min, dehydrating for 15min while exhausting air, and slowly cooling to 80 ℃ to obtain a mixture.
(3) According to the mass parts, 2 parts of dialkyl dithiocarbamate, 0.3 part of sulfurized sperm oil, 0.2 part of triethyl phosphate, 0.2 part of chlorinated paraffin, 5 parts of barium petroleum sulfonate, 1 part of sorbitol monooleate and 0.3 part of benzotriazole are sequentially added into the mixture at the temperature of 80 ℃, and the mixture is stirred for 70min at the rotating speed of 80r/min to obtain the lubricating grease.
Comparative example 1
The grease of this comparative example was prepared as follows:
1) adding 8 parts of beef tallow, 12 parts of stearic acid, 77 parts of No. 24 cylinder oil, 0.5 part of diphenylamine and 1.5 parts of sorbitan monooleate into a mixing kettle, and stirring at the temperature of 60 ℃ at the speed of 50r/min for 30min to obtain a premix;
2) dissolving 4 parts by weight of sodium hydroxide in water to obtain an alkali solution, adding the alkali solution and the premix into a reaction kettle, uniformly mixing, heating and pressurizing the reaction kettle to 150 ℃ and 0.2Mpa to perform saponification reaction for 50min, dehydrating at constant pressure for 20min, dehydrating for 10min while exhausting air, and slowly cooling to normal temperature to obtain the lubricating grease.
Comparative example 2
The grease of this comparative example was prepared as follows:
(1) adding 50 parts by mass of 46# turbine oil and 4 parts by mass of stearic acid into a reaction kettle at the temperature of 60 ℃, and stirring at the rotating speed of 60r/min for 30min to obtain a premix.
(2) Dissolving 1 part of sodium hydroxide in 2 parts of soap water according to the mass part to obtain an alkali solution; adding the alkali solution and the premix into a reaction kettle, uniformly mixing, heating and pressurizing the reaction kettle to 170 ℃ and 0.4Mpa to perform saponification reaction for 60min, dehydrating for 20min at constant pressure while exhausting air for 10min, and slowly cooling to 75 ℃ to obtain a mixture.
(3) According to the mass parts, 1 part of dialkyl dithiocarbamate, 0.2 part of sulfurized whale oil, 0.1 part of triethyl phosphate, 0.1 part of chlorinated paraffin, 3 parts of barium petroleum sulfonate and 0.5 part of sorbitol monooleate-grade 0.2 part of benzotriazole are sequentially added into the mixture at the temperature of 70 ℃, and the mixture is stirred for 60min at the rotating speed of 80r/min to obtain the lubricating grease.
And (3) testing:
1) the results of the extreme pressure measurements of the greases obtained in examples 1 to 3 and comparative examples 1 to 2 were carried out according to the method specified in GB/T12583 "method for measuring extreme pressure Performance of lubricants (four-ball method)", respectively, and are shown in Table 1.
2) The grease compositions obtained in examples 1 to 3 and comparative examples 1 to 2 were each subjected to oxidation stability measurement in accordance with the method defined in SH/T0193-92 method for measuring oxidation stability of lubricating oil (rotational oxygen bomb method), and the results are shown in Table 1.
3) The greases obtained in examples 1 to 3 and comparative examples 1 to 2 were applied to different equipment, respectively, the used greases were recovered from the equipment, and the cleanliness of the greases obtained in examples 1 to 3 and comparative examples 1 to 2 were measured according to the method specified in the national standard GB/T14039-2002 "contamination grade code for solid particles in hydraulic transmission oil", respectively, and the results are shown in Table 1.
Figure GDA0003532055870000151
As can be seen from Table 1, the greases obtained in examples 1 to 3 have higher PB value, longer oxidation stability time and higher cleanliness grade of the recovered grease oil compared with the greases obtained in comparative examples 1 to 2, which shows that the greases obtained in examples 1 to 3 have better extreme pressure property, stronger oxidation resistance and stronger capability of adsorbing fine chips and foreign matters.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (12)

1. The lubricating grease is characterized in that the lubricating grease is prepared from the following raw materials in parts by mass:
77-92 parts of base oil;
10.3 to 17.6 portions of thickening agent;
5-8 parts of a multi-metal oxygen cluster compound;
wherein the base oil comprises bio-oil and synthetic oil, and the polyoxometalate compound has a nucleophilic group and an electrophilic group.
2. The grease of claim 1, wherein the multimetal oxygen cluster compound has the formula [ Cu [ ]I(2,2'-bipy)2]{[CuI(2,2'-bipy)2]2][PW12O40]}。
3. The grease of claim 1, wherein the thickener is at least one selected from a sodium-based thickener, an aluminum-based thickener, and a lithium-based thickener.
4. The grease of claim 3, wherein the sodium-based thickener is selected from at least one of sodium sebacate and sodium salicylate; the aluminum-based thickening agent is alum; the lithium-based thickener is at least one selected from lithium 12-hydroxystearate and lithium borate.
5. The grease of claim 1, wherein the bio-oil is selected from at least one of an animal oil and a vegetable oil; and/or the synthetic oil is selected from at least one of neopentyl glycol ester, trimethylolpropane ester and pentaerythritol ester.
6. The grease of claim 1, wherein the bio-oil is selected from at least one of an animal oil and a vegetable oil selected from at least one of castor oil, sunflower oil and soybean oil; the animal oil is at least one selected from beef tallow, lard and mutton fat.
7. The lubricating grease of any one of claims 1 to 6, wherein the raw materials for preparing the lubricating grease further comprise 0.4 to 0.7 parts of an extreme pressure antiwear agent selected from at least one of sulfurized sperm oil, sulfurized olefin, triethyl phosphate, dibutyl phosphite and chlorinated paraffin.
8. The lubricating grease of any one of claims 1 to 6, wherein the raw materials for preparing the lubricating grease further comprise 1 to 2 parts of an antioxidant, and the antioxidant is selected from at least one of dialkyl dithiocarbamate, diphenylamine and N-N-butyl p-aminophenol.
9. The grease of any one of claims 1 to 6, wherein the raw materials for preparing the grease further comprise 3.5 to 6 parts of a rust inhibitor selected from at least one of barium petroleum sulfonate, calcium petroleum sulfonate, sorbitol monooleate, and sodium nitrite.
10. The lubricating grease of any one of claims 1 to 6, wherein the raw materials for preparing the lubricating grease further comprise 0.2 to 0.3 parts of a preservative selected from at least one of benzotriazole and benzothiazole.
11. A preparation method of lubricating grease is characterized by comprising the following steps:
preparing raw materials: preparing 77-92 parts of base oil, 10.3-17.6 parts of thickening agent and 5-8 parts of multi-metal oxide cluster compound according to the mass parts; wherein the base oil comprises bio-oil and synthetic oil, the polyoxometalate compound has a nucleophilic group and an electrophilic group;
mixing raw materials: mixing the base oil, the thickener and the multi-metal oxygen cluster compound at 70-80 ℃ to obtain a premix;
saponification dehydration cooling: under the conditions of 0.5MPa to 0.6MPa and 170 ℃ to 180 ℃, the pre-mixture is firstly saponified for 70min to 80min, then dehydrated for 20min to 30min under constant pressure, and then cooled to 75 ℃ to 80 ℃ to obtain the lubricating grease.
12. The method of claim 11, further comprising at least one of the following steps after the saponifying, dehydrating and cooling step:
and (3) extreme pressure antiwear treatment: firstly, adding an extreme pressure antiwear agent at 70-80 ℃, and then stirring at the rotating speed of 70-80 r/min for 60-70 min;
and (3) antioxidant treatment: firstly, adding an antioxidant at 70-80 ℃, and then stirring at a rotating speed of 70-80 r/min for 60-70 min;
and (3) rust prevention treatment: adding an antirust agent at 70-80 ℃, and then stirring at a rotating speed of 70-80 r/min for 60-70 min;
and (3) antiseptic treatment: adding preservative at 70-80 deg.c and stirring at 70-80 r/min for 60-70 min.
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