CN114381320A - Gear oil additive composition and preparation method and application thereof - Google Patents
Gear oil additive composition and preparation method and application thereof Download PDFInfo
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- CN114381320A CN114381320A CN202011135597.2A CN202011135597A CN114381320A CN 114381320 A CN114381320 A CN 114381320A CN 202011135597 A CN202011135597 A CN 202011135597A CN 114381320 A CN114381320 A CN 114381320A
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- 239000000203 mixture Substances 0.000 title claims abstract description 82
- 239000012208 gear oil Substances 0.000 title claims abstract description 63
- 239000000654 additive Substances 0.000 title claims abstract description 57
- 230000000996 additive effect Effects 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title abstract description 12
- -1 phosphate amine salt Chemical class 0.000 claims abstract description 55
- 230000002378 acidificating effect Effects 0.000 claims abstract description 33
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 26
- 239000010452 phosphate Substances 0.000 claims abstract description 26
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 229910052802 copper Inorganic materials 0.000 claims abstract description 18
- 239000010949 copper Substances 0.000 claims abstract description 18
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 15
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011593 sulfur Substances 0.000 claims abstract description 12
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 12
- 239000002199 base oil Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 claims description 11
- 239000011575 calcium Substances 0.000 claims description 8
- 229910052791 calcium Inorganic materials 0.000 claims description 8
- 150000003973 alkyl amines Chemical class 0.000 claims description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 6
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 6
- NYLJHRUQFXQNPN-UHFFFAOYSA-N 2-(tert-butyltrisulfanyl)-2-methylpropane Chemical compound CC(C)(C)SSSC(C)(C)C NYLJHRUQFXQNPN-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- BKCNDTDWDGQHSD-UHFFFAOYSA-N 2-(tert-butyldisulfanyl)-2-methylpropane Chemical compound CC(C)(C)SSC(C)(C)C BKCNDTDWDGQHSD-UHFFFAOYSA-N 0.000 claims description 3
- NHHSUCWHDQEHTJ-UHFFFAOYSA-N 2-(tert-butyltetrasulfanyl)-2-methylpropane Chemical compound CC(C)(C)SSSSC(C)(C)C NHHSUCWHDQEHTJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 claims description 3
- 229940077388 benzenesulfonate Drugs 0.000 claims description 2
- 239000003112 inhibitor Substances 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 150000003139 primary aliphatic amines Chemical class 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims 1
- 238000013268 sustained release Methods 0.000 claims 1
- 239000012730 sustained-release form Substances 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 16
- 230000007797 corrosion Effects 0.000 abstract description 14
- 239000013556 antirust agent Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 238000005461 lubrication Methods 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 13
- 238000011156 evaluation Methods 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- OOCMUZJPDXYRFD-UHFFFAOYSA-L calcium;2-dodecylbenzenesulfonate Chemical compound [Ca+2].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O.CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O OOCMUZJPDXYRFD-UHFFFAOYSA-L 0.000 description 3
- 230000001050 lubricating effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- HTDKEJXHILZNPP-UHFFFAOYSA-N dioctyl hydrogen phosphate Chemical compound CCCCCCCCOP(O)(=O)OCCCCCCCC HTDKEJXHILZNPP-UHFFFAOYSA-N 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- PXSXRABJBXYMFT-UHFFFAOYSA-N n-hexylhexan-1-amine Chemical compound CCCCCCNCCCCCC PXSXRABJBXYMFT-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C10M169/045—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution and non-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
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/02—Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds
- C10M2219/022—Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds of hydrocarbons, e.g. olefines
-
- 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
- C10M2219/10—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
- C10M2219/104—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring containing sulfur and carbon with nitrogen or oxygen in the ring
- C10M2219/106—Thiadiazoles
-
- 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
- C10M2223/043—Ammonium or amine salts thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention discloses a gear oil additive composition and a preparation method and application thereof. The gear oil additive composition comprises the following components in parts by weight based on 100 parts by weight of the composition: 70-90 parts of a sulfur-containing extreme pressure agent; 3-15 parts of an antiwear and copper slow-release agent compound; antirust agent: 0.5-5 parts. The antiwear and copper slow-release agent compound is a mixture of alkyl dithio-thiadiazole amine salt and acidic phosphate amine salt prepared by a one-step method. The gear oil additive composition is added into 85W/90 base oil according to 3.18 wt%, and the vehicle gear oil reaching GB13895-2018 specification indexes can be prepared. The gear oil additive composition has an outstanding effect on improving extreme pressure anti-wear and anti-corrosion capabilities, can effectively meet the gear lubrication requirements under extreme working conditions such as high temperature, overweight load and pitting corrosion, and is greatly reduced in additive amount compared with similar products in the market, good in economy and simple and convenient to blend.
Description
Technical Field
The invention relates to a gear oil additive composition, a preparation method and application thereof, in particular to a low-dose heavy-load vehicle gear oil additive composition, a preparation method and application thereof, and specifically relates to a gear oil additive composition containing a mixture of alkyl dithiothiadiazole amine salt and acidic phosphate amine salt as an anti-wear and copper slow-release agent.
Background
The heavy-load vehicle gear oil is mainly used for lubricating gears of a driving rear axle in a vehicle transmission system, and is particularly suitable for hyperbolic gears applied under the working conditions of high-speed impact load, high speed and low torque. In recent years, with the continuous development of automobile manufacturing industry, the gradual increase of vehicle load enables the drive axle gear to bear wider speed ratio range and larger torque, which puts higher performance requirements on gear oil, such as better bearing capacity, longer service life and lower cost. Compared with the original GB 13895-.
The ring structure of the thiadiazole compound has strong affinity to the metal surface, can prevent active sulfur and organic acid from corroding copper materials, and meanwhile, the sulfydryl substituent on the ring can improve lipophilicity, so that the additive also has good oil solubility and the function of enhancing the oil film strength, and has a positive effect of improving the extreme pressure performance of oil products. The acidic phosphate compound can severely corrode the surface due to high reactivity, generally, the corrosion of the phosphorus-containing additive to the friction surface is reduced by introducing organic amine, the reactivity of the additive is regulated, a compact adsorption film is formed on the surface of a friction pair, and the extreme pressure wear resistance is good. If the thiadiazole heterocyclic compound and the acidic phosphate amine salt can be used simultaneously in the formula of the gear oil, the synergistic effect of the thiadiazole heterocyclic compound and the acidic phosphate amine salt can be exerted to the maximum extent, the extreme pressure wear resistance of an oil product can be improved, and the corrosion of active sulfur in the oil product to nonferrous metals, particularly copper materials, can be effectively inhibited. In addition, the dosage of GL-5 heavy-load vehicle gear oil complexing agent in the current market is generally more than 3.8%, the cost is relatively high, and the low-cost requirements of the market and customers cannot be effectively met.
Disclosure of Invention
In view of the above problems, the invention provides a gear oil additive composition, a preparation method and an application thereof, wherein the gear oil additive composition adopts a novel mixture containing alkyl dithio-thiadiazole amine salt and acidic phosphate amine salt as an anti-wear and copper slow-release agent, and can simultaneously improve the extreme pressure anti-wear property and the anti-corrosion property of an oil product. The invention also provides a preparation method of the novel anti-wear and copper slow release agent and a preparation method of a heavy-duty vehicle gear oil additive composition containing the anti-wear and copper slow release agent. The gear oil additive composition of the invention is used for preparing GL-5 heavy-load vehicle gear oil with the dosage of 3.18 wt%, and the gear oil additive composition has low additive dosage and good economical efficiency.
In order to achieve the above object, the present invention provides a low-dosage heavy-duty vehicle gear oil additive composition, which comprises, based on 100 parts by weight of the gear oil additive composition:
(A) sulfur-containing extreme pressure agents: 70-90 parts;
(B) anti-wear and copper slow-release agent compound: 3-15 parts;
(C) antirust agent: 0.5-5 parts.
Preferably, the gear oil additive composition comprises the following components in parts by weight:
(A) sulfur-containing extreme pressure agents: 80-90 parts of a solvent;
(B) anti-wear and copper slow-release agent compound: 5-15 parts of a solvent;
(C) antirust agent: 1.5-5 parts.
Wherein the component (A) is at least one of high-pressure sulfurized isobutylene, di-t-butyl disulfide, di-t-butyl trisulfide and di-t-butyl tetrasulfide.
Further, the mass fraction content of sulfur element in the high-pressure sulfurized isobutylene is more than 42.5%.
Further, the component (B) is a mixture of alkyldithiothiadiazole amine salt and acidic phosphate amine salt, has the functions of resisting wear and inhibiting corrosion of copper materials, and comprises the following components in percentage by mass: 0.08-0.4% of acidic amine phosphate salt: 1.
further, the structural formula of the alkyl dithio-thiadiazole amine salt as the component (B) is as follows:
wherein R is1And R2Is C6～C18Straight or branched alkyl, R1And R2Which may be the same or different, are preferably C12～C14A tertiary alkyl group of (a); in the formula R3Is C5～C12Straight or branched chain alkyl.
Further, the structural formula of the acidic amine phosphate salt of the component (B) is as follows:
wherein R is4And R5Is C4～C12Straight-chain or branched alkyl, R4And R5Which may be the same or different, are preferably C4-C8N-alkyl of (2).
Further, the mixture of the alkyldithiothiadiazole amine salt and the acidic phosphoric ester amine salt of the component (B) can be prepared by a one-step method: 2- (C) is reacted with5～C12The alkyl dithio) -5-mercapto-1, 3, 4-thiadiazole, alkylamine and acidic phosphate react for 1.5 to 6 hours at the temperature of between 80 and 140 ℃, wherein the 2- (C)5～C12The molar ratio of the alkyl dithio) -5-mercapto-1, 3, 4-thiadiazole to the acidic phosphate ester is 0.08-0.4: 1, the molar ratio of the alkylamine to the acidic phosphate ester is 0.8-2.5: 1.
further, the alkylamine is C6～C18Straight or branched alkyl, preferably C12～C14Mixtures of isomeric primary aliphatic amines.
Preferably, the component (C) is one or more of calcium petroleum sulfonate, synthetic calcium sulfonate or calcium alkyl benzene sulfonate with a base number below 30mg KOH/g.
The invention also provides a preparation method of the gear oil additive composition, which comprises the following steps: adding the sulfur-containing extreme pressure agent as the component (A), the antiwear and copper slow-release agent compound as the component (B) and the antirust agent as the component (C) into a blending kettle at one time according to the proportion, heating and controlling the temperature at 50-65 ℃, and blending and stirring for 2-3 hours until the mixture of the component (A), the component (B) and the component (C) is completely dissolved, uniform and transparent, so as to obtain the low-dose heavy-load vehicle gear oil additive compound.
According to the application of the gear oil additive composition, the low-dosage heavy-load vehicle gear oil additive composition is added into 85W/90 base oil according to 3.18 wt%, and the vehicle gear oil meeting the GB13895-2018 specification requirement can be prepared.
In order to evaluate whether the gear oil additive composition can meet the GB13895-2018 standard after base oil is added, GB/T5906 'copper sheet corrosion test method for petroleum products', GB/T11143 'test method for antirust performance of mineral oil with an inhibitor in the presence of water', NB SH/T0518 'L-37 method for evaluating the carrying capacity of vehicle gear oil', NB SH/T0519 'evaluation method for anti-scratch performance of vehicle gear oil (L-42 method)', NB SH/T0517 'evaluation method for antirust performance of vehicle gear oil (L-33-1 method)', NB SH/T0755 'thermal oxidation evaluation method for stability of manual transmission oil and rear axle oil (L-60-1 method)', and the like are adopted for evaluation.
Compared with the prior art, the invention has the following beneficial effects:
(1) the anti-wear and copper slow-release agent compound used in the low-dose heavy-duty vehicle gear oil additive composition is a mixture of alkyldithiothiadiazole amine salt and acidic phosphate amine salt, and simultaneously improves the extreme pressure anti-wear property and the corrosion resistance of oil products.
(2) The preparation method of the acidic amine phosphate salt has been reported in related documents, but the preparation method of the alkyldithiothiadiazole amine salt has not been reported yet. The invention provides a method for preparing a mixture of alkyldithiothiadiazole amine salt and acidic phosphate amine salt by a one-step method.
(3) The gear oil additive composition is added into 85W/90 base oil according to 3.18 wt%, so that the vehicle gear oil reaching GB13895-2018 specification indexes can be prepared, the addition amount of the gear oil additive composition is greatly reduced compared with similar products in the market, the economy is good, the effect of improving extreme pressure abrasion resistance and corrosion resistance is remarkable, and the gear lubricating requirements under extreme working conditions such as high temperature, overweight load and pitting corrosion can be effectively met.
Detailed Description
The following examples of the present invention are described in detail, and the present invention is carried out on the premise of the technical scheme of the present invention, and detailed embodiments and procedures are given, but the scope of the present invention is not limited to the following examples, and the following examples are experimental methods without specific conditions noted, and generally follow conventional conditions.
Example 1:
the low-dosage heavy-duty vehicle gear oil additive composition comprises: 83.10 wt% of high-pressure sulfurized isobutylene with the sulfur element mass fraction of more than 42.5% (component A), 14.95 wt% of a mixture of alkyldithiothiadiazole amine salt and acidic phosphate amine salt (component B), and 1.95 wt% of low-base-number calcium dodecylbenzene sulfonate (component C). The sum of the above components is 100 wt%.
Example 2:
the low-dosage heavy-duty vehicle gear oil additive composition comprises: 55.55 wt% of a mixture of high-pressure sulfurized isobutylene with the sulfur element mass fraction of more than 42.5% and 30.0 wt% of di-tert-butyl trisulfide (component A), 12.5 wt% of a mixture of alkyldithiothiadiazole amine salt and acidic phosphate amine salt (component B), and 1.95 wt% of low-base-number calcium dodecylbenzene sulfonate (component C). The sum of the above components is 100 wt%.
Example 3:
the low-dosage heavy-duty vehicle gear oil additive composition comprises: 58.95 wt% of a mixture of high-pressure sulfurized isobutylene with the sulfur element mass fraction of more than 42.5% and 30.0 wt% of di-tert-butyl trisulfide (component A), 9.10 wt% of a mixture of alkyldithiothiadiazole amine salt and acidic phosphate amine salt (component B), and 1.95 wt% of low-base-number calcium dodecylbenzene sulfonate (component C). The sum of the above components is 100 wt%.
The preparation method of the mixture of the alkyldithiothiadiazole amine salt and the acidic phosphate amine salt of the component (B) in the above embodiments 1 to 3 is as follows: 27.8g of 2-tert-dodecyl-dithio-5-mercapto-1, 3, 4-thiadiazole, 194.6g of 81-R amine and 139.0g of di-n-octyl phosphate are added into a 500mL three-necked flask, and the mixture is reacted for 5 hours at 110-120 ℃ under continuous stirring. After the reaction, the system was cooled and filtered to obtain 351.1g of a mixture of 2-tert-dodecyldithio-5-mercapto-1, 3, 4-thiadiazole amine salt and di-n-octyl phosphate amine salt.
The heavy duty vehicle gear oil additive compositions of examples 1, 2 and 3 above were all added at 3.18 wt% to 85W/90 base oil, the composition and properties of which are shown in table 1, and the results of the performance tests are shown in table 2.
TABLE 185W/90 base oil composition and Properties
Table 2 results of performance tests of example 1, example 2, and example 3
The result shows that when the gear oil additive composition is added into 85W/90 base oil by 3.18 wt%, copper sheet corrosion, liquid phase corrosion and extreme pressure antiwear property of an oil product meet the index requirements. In the additive composition, the proportion of the mixture of the high-pressure sulfurized isobutylene, the alkyl dithio-thiadiazole amine salt and the acidic phosphate amine salt has great influence on copper sheet corrosion and extreme pressure abrasion resistance of an oil product. The high-pressure sulfurized isobutylene is beneficial to the extreme pressure of oil products, but can cause certain corrosion; the mixture of the alkyldithio-thiadiazole amine salt and the acidic phosphate amine salt is beneficial to the wear resistance and corrosion resistance of oil products, but has certain influence on extreme pressure, and the proportion of the alkyldithio-thiadiazole amine salt and the acidic phosphate amine salt needs to be balanced in a formula, so that the functions of extreme pressure agent high-pressure sulfurized isobutylene, wear resistance and copper slow release agent mixture of the alkyldithio-thiadiazole amine salt and the acidic phosphate amine salt are exerted to the maximum extent.
Example 4:
the low-dosage heavy-duty vehicle gear oil additive composition comprises: 55.55 wt% of high-pressure sulfurized isobutylene with the sulfur element mass fraction of more than 42.5%, 5 wt% of di-tert-butyl disulfide, 20 wt% of di-tert-butyl trisulfide, 5 wt% of di-tert-butyl tetrasulfide (component A), 12.5 wt% of mixture of alkyldithiothiadiazole amine salt and acidic phosphate amine salt (component B), 1.15 wt% of calcium petroleum sulfonate with the base number of 20-30 mg KOH/g and 0.80 wt% of synthetic calcium sulfonate (component C). The sum of the above components is 100 wt%.
The mixture of the alkyldithiothiadiazole amine salt and the acidic phosphoric acid ester amine salt of the above component (B) of example 4 is prepared as follows: 45.5g of 2-tert-octyl dithio-5-mercapto-1, 3, 4-thiadiazole, 291.2g of di-n-hexylamine and 182.0g of di-n-octyl phosphate are added into a 1000mL three-necked bottle and reacted for 4 hours at 120-130 ℃ under continuous stirring. After the reaction, the system was cooled and filtered to obtain 500.8g of a mixture of 2-tert-octyldithio-5-mercapto-1, 3, 4-thiadiazole amine salt and di-n-octyl phosphate amine salt.
The heavy duty vehicle gear oil additive compositions of example 4 above were each added at 3.18 wt% to an 85W/90 base oil, the composition and properties of which are shown in table 3, and the results of the performance tests are shown in table 4.
TABLE 385 composition and Properties of W/90 base oils
Table 4 results of performance testing of example 4
Test results show that the vehicle gear oil prepared by adding the low-dose heavy-load vehicle gear oil additive composition into 85W/90 base oil according to 3.18 wt% passes through a main rack of GL-5GB13895-2018 specification requirements, has excellent extreme pressure abrasion resistance and rust-proof corrosion resistance, and can meet the lubricating requirements of vehicle gears under extreme working conditions. Compared with the similar products in the market, the additive composition has the advantages of greatly reduced dosage, good economy and simple and convenient blending.
The present invention is capable of other embodiments, and various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (15)
1. The gear oil additive composition is characterized by comprising the following components by weight:
component (a) a sulfur-containing extreme pressure agent: 70-90 parts;
the component (B) is a compound of an antiwear and copper sustained-release agent: 3-15 parts;
component (C) rust inhibitor: 0.5-5 parts.
2. The gear oil additive composition of claim 1 wherein the component (a) is at least one of high pressure sulfurized isobutylene, di-t-butyl disulfide, di-t-butyl trisulfide and di-t-butyl tetrasulfide; the component (A) is 80-90 parts by weight.
3. The gear oil additive composition of claim 2 wherein the high pressure sulfurized isobutylene has an elemental sulfur content of greater than 42.5% by weight.
4. The gear oil additive composition of claim 1 wherein component (B) is a mixture of an alkyldithiothiadiazole amine salt and an acidic phosphate amine salt; the weight part of the component (B) is 5-15 parts.
5. The gear oil additive composition according to claim 4, wherein the component (B) is selected from the group consisting of, by mass ratio, alkyldithiothiadiazole amine salt: 0.08-0.4% of acidic amine phosphate salt: 1.
6. the gear oil additive composition of claim 5 wherein the alkyldithiothiadiazole amine salt has the structural formula:
wherein R is1And R2Is C6～C18Straight or branched alkyl, R1And R2The same or different; r3Is C5～C12Straight or branched chain alkyl.
7. The gear oil additive composition of claim 6 wherein R is1And R2Is C12～C14A tertiary alkyl group of (a).
8. The gear oil additive composition of claim 4 wherein the acidic amine phosphate salt has the formula:
wherein R is4And R5Is C4～C12Straight-chain or branched alkyl, R4And R5The same or different.
9. The gear oil additive composition of claim 8 wherein R is4And R5Is C4-C8N-alkyl of (2).
10. The gear oil additive composition of claim 4 wherein the mixture of component (B) the alkyldithiothiadiazole amine salt and the acidic phosphate amine salt is made by a one-step process comprising the steps of: 2- (C) is reacted with5～C12The alkyl dithio) -5-mercapto-1, 3, 4-thiadiazole, alkylamine and acidic phosphate react for 1.5 to 6 hours at the temperature of between 80 and 140 ℃; the 2- (C)5～C12The molar ratio of the alkyl dithio) -5-mercapto-1, 3, 4-thiadiazole to the acidic phosphate ester is 0.08-0.4: 1, the molar ratio of the alkylamine to the acidic phosphate ester is 0.8-2.5: 1.
11. the gear oil additive composition of claim 10 wherein the alkylamine is C6～C18Linear or branched alkyl groups of (1).
12. The gear oil additive composition of claim 11 wherein the alkyl amine is C12-C14Mixtures of isomeric primary aliphatic amines.
13. The gear oil additive composition of claim 1 wherein component (C) is at least one of calcium petroleum sulfonate, synthetic calcium sulfonate, and calcium alkyl benzene sulfonate having a base number of 30mg KOH/g or less; the component (C) and the component (B) account for 1.5-5 parts by weight.
14. A method of preparing the gear oil additive composition of any of claims 1-13, comprising the steps of: and adding the component (A), the component (B) and the component (C) into a blending container according to a ratio, and blending at 50-65 ℃ for 2-3 hours until the component (A), the component (B) and the component (C) are completely dissolved, uniform and transparent, so as to obtain the gear oil additive composition.
15. Use of the gear oil additive composition according to any one of claims 1 to 13, wherein the gear oil additive composition is added to 85W/90 base oil in an amount of 3.18 wt% to prepare a vehicle gear oil meeting the specification of GB 13895-2018.
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| US3519564A (en) * | 1967-08-25 | 1970-07-07 | Lubrizol Corp | Heterocyclic nitrogen-sulfur compositions and lubricants containing them |
| CA2198725A1 (en) * | 1994-08-31 | 1996-03-07 | Mobil Oil Corporation | Dimercaptothiadiazole-mercaptan coupled compounds as multifunctional additives for lubricants and fuels |
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