CN107446673B - Special protective agent for automatic start-stop and preparation method thereof - Google Patents

Special protective agent for automatic start-stop and preparation method thereof Download PDF

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CN107446673B
CN107446673B CN201710659212.4A CN201710659212A CN107446673B CN 107446673 B CN107446673 B CN 107446673B CN 201710659212 A CN201710659212 A CN 201710659212A CN 107446673 B CN107446673 B CN 107446673B
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diamond
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dopo
surface hydrophobic
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CN107446673A (en
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郝国强
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YUNHAN 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
    • C10M169/04—Mixtures of base-materials and additives
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    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
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    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/14—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
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    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/104—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only
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    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
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    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
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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
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    • 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
    • C10M2219/042—Sulfate esters
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    • 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
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    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/10—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
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    • C10M2225/00—Organic macromolecular compounds containing phosphorus as ingredients in lubricant compositions
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    • C10M2227/04—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 having a silicon-to-carbon bond, e.g. organo-silanes
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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
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Abstract

The invention discloses a special protection for automatic start-stopThe agent belongs to the technical field of automobile lubricating oil, and comprises surface hydrophobic nano diamond, lubricating grease, mineral oil, methyl silicone oil and Fe3O4The lubricant comprises powder, pentadecyl sulfonyl chloride, alcohol compounds, azole compounds, fatty glyceride, sulfate extreme pressure anti-wear agents, silane coupling agents, metal deactivators, lubrication penetrants and dispersants. The special protective agent for automatic start-stop is economical, reasonable and excellent in technology, can enable the nano-diamond to be stably dispersed in lubricating oil for a long time, reduces friction and abrasion, improves the lubricating effect, and can reduce friction heat to prevent the lubricating oil from being denatured and oxidized, so that the special protective agent has the effect of prolonging the service life of the lubricating oil, ensures the normal operation of an automobile, can effectively reduce the operation cost, is low in cost, and is economical and practical.

Description

Special protective agent for automatic start-stop and preparation method thereof
Technical Field
The invention relates to a special protective agent for automatic start-stop, in particular to a special protective agent for automatic start-stop and a preparation method thereof, belonging to the technical field of automobile lubricating oil.
Background
At present, most of lubricating oil quality is to add a plurality of organic or inorganic, liquid or solid additives to improve the performance of the lubricating oil, and realize good lubricating effect by physical or chemical adsorption and chemical reaction with the aid of the additives, and because the nano-particles have high specific surface area and unique chemical and physical properties, the nano-particles are widely valued by people in the field of new materials, and the nano-lubricating oil additives mainly comprise two types: one is Chinese patent with nano diamond as medium, such as application numbers 200410097197 and 200410067742, and the other is Chinese patent with nano copper and zinc as medium, such as application numbers 02128866, 03139679 and 03109198; the nano diamond has the advantages of excellent wear resistance and wear reduction performance, no metal ions, no toxicity and harm and poor repairing capability, the nano copper and zinc have the advantages of outstanding wear resistance and wear reduction and repairing capability and have the defects of too strong repairing capability, the places which are not repaired are also repaired, and meanwhile, the engine oil sensor fails due to the addition of metal substances, so that the problems in the use of high-grade automobiles are increased, and therefore, the special protective agent for the lubricating oil needs to be provided when the automobiles are automatically started and stopped.
Disclosure of Invention
The invention mainly aims to provide a special protective agent for automatic start-stop and a preparation method thereof, which has the advantages of simple formula, long acting and good lubricating and protecting effects.
The purpose of the invention can be achieved by adopting the following technical scheme:
a special protective agent for automatic start and stop comprises surface hydrophobic nano diamond, lubricating grease, mineral oil, methyl silicone oil and Fe3O4Powder, pentadecyl sulfonyl chloride, alcoholThe lubricating oil comprises a compound, an azole compound, fatty glyceride, a sulfate extreme pressure antiwear agent, a silane coupling agent, a metal deactivator, a lubricating penetrant and a dispersant.
Further, the special automatic start-stop protective agent comprises the following components in parts by weight: 3-5 parts of surface hydrophobic nano diamond, 10-15 parts of lubricating grease, 20-25 parts of mineral oil, 15-20 parts of methyl silicone oil and Fe3O41-2 parts of powder, 0.01-0.1 part of pentadecyl sulfonyl chloride, 1.5-2 parts of alcohol compound, 0.4-0.5 part of azole compound, 15-20 parts of fatty glyceride, 5-10 parts of sulfate extreme pressure antiwear agent, 1.5-2 parts of silane coupling agent, 1.5-3 parts of metal deactivator, 5-10 parts of lubricating penetrant and 2.5-3.5 parts of dispersant.
Further, the dispersant is an aqueous phosphorus-containing epoxy compound, the aqueous phosphorus-containing epoxy compound comprises an F-51-DOPO-MEA-PEGGE adduct, and the F-51-DOPO-MEA-PEGGE adduct is prepared by the following steps:
(1) under the molar ratio of 3:2, synthesizing an F-51-DOPO addition product by using novolac epoxy resin F-51 and DOPO,
(2): reacting the F-51-DOPO adduct with ethanolamine at a molar ratio of 1:1 to synthesize an F-51-DOPO-MEA adduct,
(3): and reacting the F-51-DOPO-MEA adduct with polyether alcohol diglycidyl ether at a molar ratio of 2:1 to synthesize the F-51-DOPO-MEA-PEGGE adduct.
Further, the surface hydrophobic nano-diamond is sulfonated surface hydrophobic polycrystalline nano-diamond, and the sulfonated surface hydrophobic polycrystalline nano-diamond is prepared by mixing the surface hydrophobic nano-diamond with 60% of H2SO4The solution is obtained after mixing and reacting at the temperature of 100 ℃.
Further, the alcohol compound is any one or a mixture of any more of methanol, ethanol, ethylene glycol and glycerol.
Further, the azole compound is any one of benzotriazole, tolyltriazole and mercaptobenzothiazole.
Furthermore, each 100 parts of the sulfate extreme pressure antiwear agent comprises 30-40 parts of pentadecyl calcium sulfate and 60-70 parts of calcium hexadecyl borate.
Further, the lubrication penetrant is any one or a mixture of any more of diethylene glycol methyl ether, polysorbate, phthalic anhydride and sebaceous acid.
Furthermore, each 100 parts of the silane coupling agent comprises 60-70 parts of hexadecyl trimethoxy silane and 30-40 parts of dodecyl trimethoxy silane.
A preparation method of a special protective agent for automatic start and stop comprises the following steps:
step 1: mixing surface hydrophobic nano diamond and Fe3O4Powder with 60% H2SO4The solution is mixed and reacted at the temperature of 100 ℃ to obtain sulfonated surface hydrophobic polycrystalline nano-diamond;
step 2: selecting sulfonated surface hydrophobic polycrystalline nano-diamond, putting the sulfonated surface hydrophobic polycrystalline nano-diamond into a reaction vessel, and adding deionized water into the reaction vessel to obtain a clear solution;
and step 3: putting the clarified solution into an ultrasonic disperser, processing by the ultrasonic disperser to obtain a nano-diamond aqueous solution, and adding an alcohol compound, an azole compound and fatty glyceride into the diamond aqueous solution to obtain a mixed solution;
and 4, step 4: screening the obtained mixed solution by a centrifugal machine to obtain a mixture;
and 5: adding the screened mixture into a mixed solution of lubricating grease, mineral oil, methyl silicone oil and pentadecyl sulfonyl chloride, and preparing into a mixed solution after 30 min;
step 6: and (5) adding a silane coupling agent, a metal deactivator, a lubricating penetrant and a dispersant into the mixed solution in the step (5), and performing ultrasonic dispersion for 60min to prepare the special automatic start-stop protective agent.
The invention has the beneficial technical effects that: according to the special protective agent for automatic start-stop and the preparation method thereof, the special protective agent for automatic start-stop and the preparation method thereof provided by the invention are economical, reasonable and excellent in technology, can ensure that the nano-diamond is stably dispersed in the lubricating oil for a long time, and reduce friction and abrasion, thereby improving the lubricating effect, and can also reduce friction heat to prevent the lubricating oil from being denatured and oxidized, thereby having the effect of prolonging the service life of the lubricating oil, ensuring the normal operation of an automobile and effectively reducing the operation cost, and the protective agent is low in cost, economical and practical.
Detailed Description
In order to make the technical solutions of the present invention more clear and definite for those skilled in the art, the present invention is further described in detail with reference to the following examples, but the embodiments of the present invention are not limited thereto.
Example 1:
the automatic start-stop special protective agent provided by the embodiment 1 comprises surface hydrophobic nano-diamond, lubricating grease, mineral oil, methyl silicone oil and Fe3O4The lubricant comprises powder, pentadecyl sulfonyl chloride, alcohol compounds, azole compounds, fatty glyceride, sulfate extreme pressure anti-wear agents, silane coupling agents, metal deactivators, lubrication penetrants and dispersants.
Further, in this embodiment 1, the protection agent specially used for automatic start-stop includes the following components by weight: 3 parts of surface hydrophobic nano-diamond, lubricating grease, mineral oil, 30 parts of methyl silicone oil, 0.01 part of pentadecyl sulfonyl chloride, 1.5 parts of alcohol compound, 0.4 part of azole compound, 15 parts of fatty glyceride, 5 parts of sulfate extreme pressure antiwear agent, 1.5 parts of silane coupling agent, 1.5 parts of metal deactivator, 5 parts of lubricating penetrant and 2.5 parts of dispersant.
Further, in this example 1, the dispersant is an aqueous phosphorus-containing epoxy compound comprising an F-51-DOPO-MEA-PEGGE adduct, and the F-51-DOPO-MEA-PEGGE adduct is prepared as follows:
(1) under the molar ratio of 3:2, synthesizing an F-51-DOPO addition product by using novolac epoxy resin F-51 and DOPO,
(2): reacting the F-51-DOPO adduct with ethanolamine at a molar ratio of 1:1 to synthesize an F-51-DOPO-MEA adduct,
(3): and reacting the F-51-DOPO-MEA adduct with polyether alcohol diglycidyl ether at a molar ratio of 2:1 to synthesize the F-51-DOPO-MEA-PEGGE adduct.
Further, in this example 1, the surface hydrophobic nanodiamond was a sulfonated surface hydrophobic polycrystalline nanodiamond by mixing the surface hydrophobic nanodiamond with 60% H2SO4The solution is obtained after mixing reaction at the temperature of 100 ℃, and the alcohol compound is any one or mixture of any more of methanol, ethanol, glycol and glycerol; the azole compound is any one of benzotriazole, methyl benzotriazole and mercapto benzothiazole.
Further, in this embodiment 1, each 100 parts of the sulfate extreme pressure antiwear agent includes 30 to 40 parts of pentadecyl calcium sulfate and 60 to 70 parts of calcium hexadecyl borate; the lubrication penetrant is any one or a mixture of any more of diethylene glycol-methyl ether, polysorbate, phthalic anhydride and sebacylic acid; every 100 parts of the silane coupling agent comprises 60-70 parts of hexadecyl trimethoxy silane and 30-40 parts of dodecyl trimethoxy silane.
The preparation method of the special protective agent for automatic start and stop provided by this embodiment 1 includes the following steps:
step 1: mixing surface hydrophobic nano diamond and Fe3O4Powder with 60% H2SO4The solution is mixed and reacted at the temperature of 100 ℃ to obtain sulfonated surface hydrophobic polycrystalline nano-diamond;
step 2: selecting sulfonated surface hydrophobic polycrystalline nano-diamond, putting the sulfonated surface hydrophobic polycrystalline nano-diamond into a reaction vessel, and adding deionized water into the reaction vessel to obtain a clear solution;
and step 3: putting the clarified solution into an ultrasonic disperser, processing by the ultrasonic disperser to obtain a nano-diamond aqueous solution, and adding an alcohol compound, an azole compound and fatty glyceride into the diamond aqueous solution to obtain a mixed solution;
and 4, step 4: screening the obtained mixed solution by a centrifugal machine to obtain a mixture;
and 5: adding the screened mixture into a mixed solution of lubricating grease, mineral oil, methyl silicone oil and pentadecyl sulfonyl chloride, and preparing into a mixed solution after 30 min;
step 6: and (5) adding a silane coupling agent, a metal deactivator, a lubricating penetrant and a dispersant into the mixed solution in the step (5), and performing ultrasonic dispersion for 60min to prepare the special automatic start-stop protective agent.
Example 2:
the automatic start-stop special protective agent provided by the embodiment 2 comprises surface hydrophobic nano-diamond, lubricating grease, mineral oil, methyl silicone oil and Fe3O4The lubricant comprises powder, pentadecyl sulfonyl chloride, alcohol compounds, azole compounds, fatty glyceride, sulfate extreme pressure anti-wear agents, silane coupling agents, metal deactivators, lubrication penetrants and dispersants.
Further, in this embodiment 2, the protection agent specially used for automatic start-stop includes the following components by weight: 3.5 parts of surface hydrophobic nano-diamond, lubricating grease, mineral oil, 35 parts of methyl silicone oil, 0.03 part of pentadecyl sulfonyl chloride, 1.6 parts of alcohol compound, 0.45 part of azole compound, 16 parts of fatty glyceride, 6 parts of sulfate extreme pressure antiwear agent, 1.6 parts of silane coupling agent, 1.8 parts of metal deactivator, 6 parts of lubricating penetrant and 2.8 parts of dispersant.
Further, in this example 2, the dispersant is an aqueous phosphorus-containing epoxy compound comprising an F-51-DOPO-MEA-PEGGE adduct, and the F-51-DOPO-MEA-PEGGE adduct is prepared as follows:
(1) under the molar ratio of 3:2, synthesizing an F-51-DOPO addition product by using novolac epoxy resin F-51 and DOPO,
(2): reacting the F-51-DOPO adduct with ethanolamine at a molar ratio of 1:1 to synthesize an F-51-DOPO-MEA adduct,
(3): and reacting the F-51-DOPO-MEA adduct with polyether alcohol diglycidyl ether at a molar ratio of 2:1 to synthesize the F-51-DOPO-MEA-PEGGE adduct.
Further, in this example 2, the surface hydrophobic nanodiamond was a sulfonated surface hydrophobic polycrystalline nanodiamond by mixing the surface hydrophobic nanodiamond with 60% H2SO4The solution is obtained after mixing reaction at the temperature of 100 ℃; the alcohol compound is any one or a mixture of any more of methanol, ethanol, glycol and glycerol; the azole compound is any one of benzotriazole, methyl benzotriazole and mercapto benzothiazole.
Further, in this embodiment 2, each 100 parts of the sulfate extreme pressure antiwear agent includes 30 to 40 parts of pentadecyl calcium sulfate and 60 to 70 parts of calcium hexadecyl borate; the lubrication penetrant is any one or a mixture of any more of diethylene glycol-methyl ether, polysorbate, phthalic anhydride and sebacylic acid; every 100 parts of the silane coupling agent comprises 60-70 parts of hexadecyl trimethoxy silane and 30-40 parts of dodecyl trimethoxy silane.
The preparation method of the special protective agent for automatic start-stop provided by embodiment 2 includes the following steps:
step 1: mixing surface hydrophobic nano diamond and Fe3O4Powder with 60% H2SO4The solution is mixed and reacted at the temperature of 100 ℃ to obtain sulfonated surface hydrophobic polycrystalline nano-diamond;
step 2: selecting sulfonated surface hydrophobic polycrystalline nano-diamond, putting the sulfonated surface hydrophobic polycrystalline nano-diamond into a reaction vessel, and adding deionized water into the reaction vessel to obtain a clear solution;
and step 3: putting the clarified solution into an ultrasonic disperser, processing by the ultrasonic disperser to obtain a nano-diamond aqueous solution, and adding an alcohol compound, an azole compound and fatty glyceride into the diamond aqueous solution to obtain a mixed solution;
and 4, step 4: screening the obtained mixed solution by a centrifugal machine to obtain a mixture;
and 5: adding the screened mixture into a mixed solution of lubricating grease, mineral oil, methyl silicone oil and pentadecyl sulfonyl chloride, and preparing into a mixed solution after 30 min;
step 6: and (5) adding a silane coupling agent, a metal deactivator, a lubricating penetrant and a dispersant into the mixed solution in the step (5), and performing ultrasonic dispersion for 60min to prepare the special automatic start-stop protective agent.
Example 3:
the automatic start-stop special protective agent provided by the embodiment 3 comprises surface hydrophobic nano-diamond, lubricating grease, mineral oil, methyl silicone oil and Fe3O4The lubricant comprises powder, pentadecyl sulfonyl chloride, alcohol compounds, azole compounds, fatty glyceride, sulfate extreme pressure anti-wear agents, silane coupling agents, metal deactivators, lubrication penetrants and dispersants.
Further, in this embodiment 3, the protection agent specially used for automatic start-stop includes the following components by weight: 4 parts of surface hydrophobic nano-diamond, lubricating grease, mineral oil, 40 parts of methyl silicone oil, 0.05 part of pentadecyl sulfonyl chloride, 1.7 parts of alcohol compounds, 0.45 part of azole compounds, 17 parts of fatty glyceride, 7 parts of sulfate extreme pressure antiwear agent, 1.7 parts of silane coupling agent, 2 parts of metal deactivator, 7 parts of lubricating penetrant and 2.9 parts of dispersant.
Further, in this example 3, the dispersant is an aqueous phosphorus-containing epoxy compound comprising an F-51-DOPO-MEA-PEGGE adduct, and the F-51-DOPO-MEA-PEGGE adduct is prepared as follows:
(1) under the molar ratio of 3:2, synthesizing an F-51-DOPO addition product by using novolac epoxy resin F-51 and DOPO,
(2): reacting the F-51-DOPO adduct with ethanolamine at a molar ratio of 1:1 to synthesize an F-51-DOPO-MEA adduct,
(3): and reacting the F-51-DOPO-MEA adduct with polyether alcohol diglycidyl ether at a molar ratio of 2:1 to synthesize the F-51-DOPO-MEA-PEGGE adduct.
Further, in this example 3, the surface hydrophobic nanodiamond is sulfonated surface hydrophobic polycrystalineThe sulfonated surface hydrophobic polycrystalline nano-diamond is prepared by mixing surface hydrophobic nano-diamond with 60% H2SO4The solution is obtained after mixing reaction at the temperature of 100 ℃; the alcohol compound is any one or a mixture of any more of methanol, ethanol, glycol and glycerol; the azole compound is any one of benzotriazole, methyl benzotriazole and mercapto benzothiazole.
Further, in this embodiment 3, each 100 parts of the sulfate extreme pressure antiwear agent includes 30 to 40 parts of pentadecyl calcium sulfate and 60 to 70 parts of calcium hexadecyl borate; the lubrication penetrant is any one or a mixture of any more of diethylene glycol-methyl ether, polysorbate, phthalic anhydride and sebacylic acid; every 100 parts of the silane coupling agent comprises 60-70 parts of hexadecyl trimethoxy silane and 30-40 parts of dodecyl trimethoxy silane.
The preparation method of the special protective agent for automatic start-stop provided by this embodiment 3 includes the following steps:
step 1: mixing surface hydrophobic nano diamond and Fe3O4Powder with 60% H2SO4The solution is mixed and reacted at the temperature of 100 ℃ to obtain sulfonated surface hydrophobic polycrystalline nano-diamond;
step 2: selecting sulfonated surface hydrophobic polycrystalline nano-diamond, putting the sulfonated surface hydrophobic polycrystalline nano-diamond into a reaction vessel, and adding deionized water into the reaction vessel to obtain a clear solution;
and step 3: putting the clarified solution into an ultrasonic disperser, processing by the ultrasonic disperser to obtain a nano-diamond aqueous solution, and adding an alcohol compound, an azole compound and fatty glyceride into the diamond aqueous solution to obtain a mixed solution;
and 4, step 4: screening the obtained mixed solution by a centrifugal machine to obtain a mixture;
and 5: adding the screened mixture into a mixed solution of lubricating grease, mineral oil, methyl silicone oil and pentadecyl sulfonyl chloride, and preparing into a mixed solution after 30 min;
step 6: and (5) adding a silane coupling agent, a metal deactivator, a lubricating penetrant and a dispersant into the mixed solution in the step (5), and performing ultrasonic dispersion for 60min to prepare the special automatic start-stop protective agent.
Example 4:
the automatic start-stop special protective agent provided by the embodiment 4 comprises surface hydrophobic nano-diamond, lubricating grease, mineral oil, methyl silicone oil and Fe3O4The lubricant comprises powder, pentadecyl sulfonyl chloride, alcohol compounds, azole compounds, fatty glyceride, sulfate extreme pressure anti-wear agents, silane coupling agents, metal deactivators, lubrication penetrants and dispersants.
Further, in this embodiment 4, the protection agent specially used for automatic start-stop includes the following components by weight: 4.2 parts of surface hydrophobic nano-diamond, lubricating grease, mineral oil, 45 parts of methyl silicone oil, 0.07 part of pentadecyl sulfonyl chloride, 1.8 parts of alcohol compound, 0.45 part of azole compound, 18 parts of fatty glyceride, 8 parts of sulfate extreme pressure antiwear agent, 1.8 parts of silane coupling agent, 2.5 parts of metal deactivator, 8 parts of lubricating penetrant and 3.2 parts of dispersant.
Further, in this example 4, the dispersant is an aqueous phosphorus-containing epoxy compound comprising an F-51-DOPO-MEA-PEGGE adduct, and the F-51-DOPO-MEA-PEGGE adduct is prepared as follows:
(1) under the molar ratio of 3:2, synthesizing an F-51-DOPO addition product by using novolac epoxy resin F-51 and DOPO,
(2): reacting the F-51-DOPO adduct with ethanolamine at a molar ratio of 1:1 to synthesize an F-51-DOPO-MEA adduct,
(3): and reacting the F-51-DOPO-MEA adduct with polyether alcohol diglycidyl ether at a molar ratio of 2:1 to synthesize the F-51-DOPO-MEA-PEGGE adduct.
Further, in this example 4, the surface hydrophobic nanodiamond was a sulfonated surface hydrophobic polycrystalline nanodiamond by mixing the surface hydrophobic nanodiamond with 60% H2SO4The solution is at 100 deg.CObtained after mixing reaction under the condition of certain degree; the alcohol compound is any one or a mixture of any more of methanol, ethanol, glycol and glycerol; the azole compound is any one of benzotriazole, methyl benzotriazole and mercapto benzothiazole.
Further, in this embodiment 4, each 100 parts of the sulfate extreme pressure antiwear agent includes 30 to 40 parts of pentadecyl calcium sulfate and 60 to 70 parts of calcium hexadecyl borate; the lubrication penetrant is any one or a mixture of any more of diethylene glycol-methyl ether, polysorbate, phthalic anhydride and sebacylic acid; every 100 parts of the silane coupling agent comprises 60-70 parts of hexadecyl trimethoxy silane and 30-40 parts of dodecyl trimethoxy silane.
The preparation method of the special protective agent for automatic start and stop provided by this embodiment 4 includes the following steps:
step 1: mixing surface hydrophobic nano diamond and Fe3O4Powder with 60% H2SO4The solution is mixed and reacted at the temperature of 100 ℃ to obtain sulfonated surface hydrophobic polycrystalline nano-diamond;
step 2: selecting sulfonated surface hydrophobic polycrystalline nano-diamond, putting the sulfonated surface hydrophobic polycrystalline nano-diamond into a reaction vessel, and adding deionized water into the reaction vessel to obtain a clear solution;
and step 3: putting the clarified solution into an ultrasonic disperser, processing by the ultrasonic disperser to obtain a nano-diamond aqueous solution, and adding an alcohol compound, an azole compound and fatty glyceride into the diamond aqueous solution to obtain a mixed solution;
and 4, step 4: screening the obtained mixed solution by a centrifugal machine to obtain a mixture;
and 5: adding the screened mixture into a mixed solution of lubricating grease, mineral oil, methyl silicone oil and pentadecyl sulfonyl chloride, and preparing into a mixed solution after 30 min;
step 6: and (5) adding a silane coupling agent, a metal deactivator, a lubricating penetrant and a dispersant into the mixed solution in the step (5), and performing ultrasonic dispersion for 60min to prepare the special automatic start-stop protective agent.
Example 5:
the automatic start-stop special protective agent provided by the embodiment 5 comprises surface hydrophobic nano-diamond, lubricating grease, mineral oil, methyl silicone oil and Fe3O4The lubricant comprises powder, pentadecyl sulfonyl chloride, alcohol compounds, azole compounds, fatty glyceride, sulfate extreme pressure anti-wear agents, silane coupling agents, metal deactivators, lubrication penetrants and dispersants.
Further, in this embodiment 5, the protection agent specially used for automatic start-stop includes the following components by weight: 4.8 parts of surface hydrophobic nano-diamond, lubricating grease, mineral oil, 48 parts of methyl silicone oil, 0.09 part of pentadecyl sulfonyl chloride, 1.9 parts of alcohol compound, 0.45 part of azole compound, 19 parts of fatty glyceride, 9 parts of sulfate extreme pressure antiwear agent, 1.9 parts of silane coupling agent, 2.8 parts of metal deactivator, 9 parts of lubricating penetrant and 3.4 parts of dispersant.
Further, in this example 5, the dispersant is an aqueous phosphorus-containing epoxy compound comprising an F-51-DOPO-MEA-PEGGE adduct, and the F-51-DOPO-MEA-PEGGE adduct is prepared as follows:
(1) under the molar ratio of 3:2, synthesizing an F-51-DOPO addition product by using novolac epoxy resin F-51 and DOPO,
(2): reacting the F-51-DOPO adduct with ethanolamine at a molar ratio of 1:1 to synthesize an F-51-DOPO-MEA adduct,
(3): and reacting the F-51-DOPO-MEA adduct with polyether alcohol diglycidyl ether at a molar ratio of 2:1 to synthesize the F-51-DOPO-MEA-PEGGE adduct.
Further, in this example 5, the surface hydrophobic nanodiamonds were sulfonated surface hydrophobic polycrystalline nanodiamonds by mixing the surface hydrophobic nanodiamonds with 60% H2SO4The solution is obtained after mixing reaction at the temperature of 100 ℃; the alcohol compound is any one or a mixture of any more of methanol, ethanol, glycol and glycerol; what is needed isThe azole compound is any one of benzotriazole, tolyltriazole and mercapto benzothiazole.
Further, in this example 5, each 100 parts of the sulfate extreme pressure antiwear agent includes 30 to 40 parts of pentadecyl calcium sulfate and 60 to 70 parts of calcium hexadecyl borate; the lubrication penetrant is any one or a mixture of any more of diethylene glycol-methyl ether, polysorbate, phthalic anhydride and sebacylic acid; every 100 parts of the silane coupling agent comprises 60-70 parts of hexadecyl trimethoxy silane and 30-40 parts of dodecyl trimethoxy silane.
The preparation method of the special protective agent for automatic start-stop provided by this embodiment 5 includes the following steps:
step 1: mixing surface hydrophobic nano diamond and Fe3O4Powder with 60% H2SO4The solution is mixed and reacted at the temperature of 100 ℃ to obtain sulfonated surface hydrophobic polycrystalline nano-diamond;
step 2: selecting sulfonated surface hydrophobic polycrystalline nano-diamond, putting the sulfonated surface hydrophobic polycrystalline nano-diamond into a reaction vessel, and adding deionized water into the reaction vessel to obtain a clear solution;
and step 3: putting the clarified solution into an ultrasonic disperser, processing by the ultrasonic disperser to obtain a nano-diamond aqueous solution, and adding an alcohol compound, an azole compound and fatty glyceride into the diamond aqueous solution to obtain a mixed solution;
and 4, step 4: screening the obtained mixed solution by a centrifugal machine to obtain a mixture;
and 5: adding the screened mixture into a mixed solution of lubricating grease, mineral oil, methyl silicone oil and pentadecyl sulfonyl chloride, and preparing into a mixed solution after 30 min;
step 6: and (5) adding a silane coupling agent, a metal deactivator, a lubricating penetrant and a dispersant into the mixed solution in the step (5), and performing ultrasonic dispersion for 60min to prepare the special automatic start-stop protective agent.
Example 6:
the protecting agent special for automatic start and stop provided by the embodiment 6 comprisesSurface hydrophobic nano diamond, lubricating grease, mineral oil, methyl silicone oil and Fe3O4The lubricant comprises powder, pentadecyl sulfonyl chloride, alcohol compounds, azole compounds, fatty glyceride, sulfate extreme pressure anti-wear agents, silane coupling agents, metal deactivators, lubrication penetrants and dispersants.
Further, in this embodiment 6, the protection agent specially used for automatic start-stop includes the following components by weight: 5 parts of surface hydrophobic nano-diamond, 50 parts of lubricating grease, mineral oil, 50 parts of methyl silicone oil, 0.1 part of pentadecyl sulfonyl chloride, 2 parts of alcohol compounds, 0.5 part of azole compounds, 20 parts of fatty glyceride, 10 parts of sulfate extreme pressure antiwear agent, 2 parts of silane coupling agent, 3 parts of metal deactivator, 10 parts of lubricating penetrant and 3.5 parts of dispersing agent.
Further, in this example 6, the dispersant is an aqueous phosphorus-containing epoxy compound comprising an F-51-DOPO-MEA-PEGGE adduct, and the F-51-DOPO-MEA-PEGGE adduct is prepared as follows:
(1) under the molar ratio of 3:2, synthesizing an F-51-DOPO addition product by using novolac epoxy resin F-51 and DOPO,
(2): reacting the F-51-DOPO adduct with ethanolamine at a molar ratio of 1:1 to synthesize an F-51-DOPO-MEA adduct,
(3): and reacting the F-51-DOPO-MEA adduct with polyether alcohol diglycidyl ether at a molar ratio of 2:1 to synthesize the F-51-DOPO-MEA-PEGGE adduct.
Further, in this example 6, the surface hydrophobic nanodiamonds were sulfonated surface hydrophobic polycrystalline nanodiamonds by mixing the surface hydrophobic nanodiamonds with 60% H2SO4The solution is obtained after mixing reaction at the temperature of 100 ℃; the alcohol compound is any one or a mixture of any more of methanol, ethanol, glycol and glycerol; the azole compound is any one of benzotriazole, methyl benzotriazole and mercapto benzothiazole.
Further, in this example 6, each 100 parts of the sulfate extreme pressure antiwear agent includes 30 to 40 parts of pentadecyl calcium sulfate and 60 to 70 parts of calcium hexadecyl borate; the lubrication penetrant is any one or a mixture of any more of diethylene glycol-methyl ether, polysorbate, phthalic anhydride and sebacylic acid; every 100 parts of the silane coupling agent comprises 60-70 parts of hexadecyl trimethoxy silane and 30-40 parts of dodecyl trimethoxy silane.
The preparation method of the special protective agent for automatic start and stop provided by this embodiment 6 includes the following steps:
step 1: mixing surface hydrophobic nano diamond and Fe3O4Powder with 60% H2SO4The solution is mixed and reacted at the temperature of 100 ℃ to obtain sulfonated surface hydrophobic polycrystalline nano-diamond;
step 2: selecting sulfonated surface hydrophobic polycrystalline nano-diamond, putting the sulfonated surface hydrophobic polycrystalline nano-diamond into a reaction vessel, and adding deionized water into the reaction vessel to obtain a clear solution;
and step 3: putting the clarified solution into an ultrasonic disperser, processing by the ultrasonic disperser to obtain a nano-diamond aqueous solution, and adding an alcohol compound, an azole compound and fatty glyceride into the diamond aqueous solution to obtain a mixed solution;
and 4, step 4: screening the obtained mixed solution by a centrifugal machine to obtain a mixture;
and 5: adding the screened mixture into a mixed solution of lubricating grease, mineral oil, methyl silicone oil and pentadecyl sulfonyl chloride, and preparing into a mixed solution after 30 min;
step 6: and (5) adding a silane coupling agent, a metal deactivator, a lubricating penetrant and a dispersant into the mixed solution in the step (5), and performing ultrasonic dispersion for 60min to prepare the special automatic start-stop protective agent.
In summary, in embodiments 1 to 4, according to the automatic start-stop dedicated protective agent and the preparation method thereof of embodiments 1 to 4, and the automatic start-stop dedicated protective agent and the preparation method thereof provided in embodiments 1 to 4, the automatic start-stop dedicated protective agent is economical and reasonable, has excellent technology, can stably disperse the nano-diamond in the lubricating oil for a long time, and reduces friction and wear, thereby improving the lubricating effect, and can also reduce friction heat to prevent the lubricating oil from being denatured and oxidized, thereby having the effect of improving the service life of the lubricating oil, ensuring the normal operation of the automobile, and effectively reducing the operation cost, and the protective agent is low in cost, economical and practical.
The above description is only for the purpose of illustrating the present invention and is not intended to limit the scope of the present invention, and any person skilled in the art can substitute or change the technical solution of the present invention and its conception within the scope of the present invention.

Claims (6)

1. The special protective agent for automatic start and stop is characterized by comprising the following components in parts by weight: 3-5 parts of surface hydrophobic nano diamond, 10-15 parts of lubricating grease, 20-25 parts of mineral oil, 15-20 parts of methyl silicone oil and Fe3O41-2 parts of powder, 0.01-0.1 part of pentadecyl sulfonyl chloride, 1.5-2 parts of alcohol compound, 0.4-0.5 part of azole compound, 15-20 parts of fatty glyceride, 5-10 parts of sulfate extreme pressure antiwear agent, 1.5-2 parts of silane coupling agent, 1.5-3 parts of metal deactivator, 5-10 parts of lubricating penetrant and 2.5-3.5 parts of dispersant; wherein the dispersant is a water-based phosphorus-containing epoxy compound, the water-based phosphorus-containing epoxy compound comprises an F-51-DOPO-MEA-PEGGE adduct, and the preparation process of the F-51-DOPO-MEA-PEGGE adduct comprises the following steps:
(1) under the molar ratio of 3:2, synthesizing an F-51-DOPO addition product by using novolac epoxy resin F-51 and DOPO,
(2): reacting the F-51-DOPO adduct with ethanolamine at a molar ratio of 1:1 to synthesize an F-51-DOPO-MEA adduct,
(3): reacting the F-51-DOPO-MEA addition product with polyether alcohol diglycidyl ether at the molar ratio of 2:1 to synthesize an addition product containing F-51-DOPO-MEA-PEGGE;
the surface hydrophobic nano-diamond is sulfonated surface hydrophobic polycrystalline nano-diamond, and the sulfonated surface hydrophobic polycrystalline nano-diamond is formed by combining the surface of the nano-diamond with the surface hydrophobic polycrystalline nano-diamondHydrophobic nanodiamond with 60% H2SO4The solution is obtained after mixing reaction at the temperature of 100 ℃;
the preparation method of the special protective agent for automatic start and stop comprises the following steps:
step 1: mixing surface hydrophobic nano diamond and Fe3O4Powder with 60% H2SO4The solution is mixed and reacted at the temperature of 100 ℃ to obtain sulfonated surface hydrophobic polycrystalline nano-diamond;
step 2: selecting sulfonated surface hydrophobic polycrystalline nano-diamond, putting the sulfonated surface hydrophobic polycrystalline nano-diamond into a reaction vessel, and adding deionized water into the reaction vessel to obtain a clear solution;
and step 3: putting the clarified solution into an ultrasonic disperser, processing by the ultrasonic disperser to obtain a nano-diamond aqueous solution, and adding an alcohol compound, an azole compound and fatty glyceride into the diamond aqueous solution to obtain a mixed solution;
and 4, step 4: screening the obtained mixed solution by a centrifugal machine to obtain a mixture;
and 5: adding the screened mixture into a mixed solution of lubricating grease, mineral oil, methyl silicone oil and pentadecyl sulfonyl chloride, and preparing into a mixed solution after 30 min;
step 6: and (5) adding a silane coupling agent, a metal deactivator, a lubricating penetrant and a dispersant into the mixed solution in the step (5), and performing ultrasonic dispersion for 60min to prepare the special automatic start-stop protective agent.
2. The special automatic start-stop protective agent according to claim 1, wherein the alcohol compound is any one or a mixture of any more of methanol, ethanol, ethylene glycol and glycerol.
3. The special automatic start-stop protective agent according to claim 1, wherein the azole compound is any one of benzotriazole, tolyltriazole and mercaptobenzothiazole.
4. The special automatic start-stop protective agent according to claim 1, wherein each 100 parts of the sulfate extreme pressure antiwear agent comprises 30-40 parts of pentadecyl calcium sulfate and 60-70 parts of hexadecyl calcium borate.
5. The special automatic start-stop protective agent according to claim 1, wherein the lubricating penetrant is any one or a mixture of any more of diethylene glycol methyl ether, polysorbate, phthalic anhydride and sebacylic acid.
6. The special protective agent for automatic start-stop according to claim 1, wherein each 100 parts of the silane coupling agent comprises 60-70 parts of hexadecyl trimethoxy silane and 30-40 parts of dodecyl trimethoxy silane.
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