CN1138086A - Additive for lubricating oil - Google Patents
Additive for lubricating oil Download PDFInfo
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- CN1138086A CN1138086A CN 96104720 CN96104720A CN1138086A CN 1138086 A CN1138086 A CN 1138086A CN 96104720 CN96104720 CN 96104720 CN 96104720 A CN96104720 A CN 96104720A CN 1138086 A CN1138086 A CN 1138086A
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Abstract
The additive for lubricant oil is prepared from MoO3, sodium hydroxide, WO3, sodium sulfide/sodium hydrogen sulfide, diisooctyl dithiophosphoric acid, sulfuric acid, basic oil 150SN of lubricant, zinc dialkylthiophosphorate and unsaturated butandioic acid through reaction, extraction, water washing, deposition separation, crystallizing, filtering and blending, and features complete and strong functions, and high effect.
Description
The invention belongs to the field of lubricating oil additives, and particularly relates to an antifriction, antiwear and energy-saving lubricating oil additive and a preparation method thereof, wherein the international patent classification number is C10M 139/00.
It is known that the antifriction, antiwear and energy-saving lubricating oil additive is actively researched and developed in the United states, Japan, West Germany, France, Su Union and China, MODTP produced in Japan is also called oil-soluble organic molybdenum as a well-known antiwear agent with a great development prospect, but is actually a substance suspended in base oil, which is insoluble in oil and often blocks a filter screen in the using process; the research, development and popularization of MODTP in the United states begin early, particularly Vanderbit company gets better, because the price is expensive and can only be accepted by high-grade lubricating oil company, the Wanji Ling product developed in Guangxi Zhongshan of China is MODTP with international level, the solubility of the product in oil is better than that of Japanese MODTP, but the product has serious pollution in the production process, has offensive odor causing nausea and dizziness, has high cost, influences the popularization and application of the product, and is recorded by documents: the production method of dialkyl dithiophosphate is characterized by that the alcohol and phosphorus pentoxide are undergone the process of sulfur-phosphorus reaction, in the course of said reaction a large quantity of hydrogen sulfide is produced, and the affinity of unreacted alcohol and reaction product is strong, so that it is difficult to separate alcohol from product by using general separation method, so that the product has the bad smell.
The invention aims to provide a preparation method for eliminating environmental pollution, reducing production cost, improving the performance of products safely and reliably, and the produced high-grade extreme pressure anti-wear lubricating oil additive has the advantages of friction reduction, wear resistance, energy conservation, elimination of the odor of the products and increase of the oil solubility of MODTP.
The purpose of the invention is realized as follows: 25-35 parts of molybdenum trioxide, 4-8 parts of sodium hydroxide and water enter a reactor (1), the reactor (1) is a molybdate and tungstate generator which reacts for 0.5-1.0 hour at normal temperature and pressure to generate sodium molybdate, 1-4 parts of tungsten trioxide is added during the reaction and continuously reacts for 0.5-1.0 hour to generate sodium tungstate by continuous stirring, then 1-4 parts of sodium sulfide or sodium hydrosulfide are added to generate a mixture of sodium molybdate sulfide and sodium tungstate sulfide, the mixture reacts for 0.5-1.0 hour and enters a second reactor (2) which is an extraction reactor, 140 parts of diisooctyl dithiophosphoric acid and 2-12 parts of sulfuric acid or hydrochloric acid or acetic acid are added as catalysts, nitrogen is introduced, 3-10 parts of lubricating oil base oil 150SN is added, and the reaction is carried out for 3-5 hours at 80-100 ℃, the obtained liquid product emits a small amount of hydrogen sulfide gas, sodium hydroxide is used for absorbing the hydrogen sulfide gas, sodium sulfide or sodium hydrosulfide is obtained after refining and is circulated to a reactor (1) for reuse, the liquid product is washed by water, settled and separated, crystallized and filtered to obtain molybdenum sulfide and tungsten sulfide (A) of the diisooctyl dithiophosphate, zinc dialkyl dithiophosphate (B) is added, the ratio of A to B is 0: 5 (weight parts are 0-700), and 5-600ppm of unsaturated succinic acid is added for blending to prepare the lubricating oil additive, wherein the main element contained in the lubricating oil additive accounts for 1.0-9.0 percent of molybdenum in the weight percentage of the lubricating oil additive; tungsten is 700 + 10000 ppm; 0-6.5% of zinc and 5-600ppm of unsaturated succinic acid.
The invention adopts diisooctyl dithiophosphate as the raw material, which not only greatly improves the solubility of the additive, but also eliminates the odor of the product. The chemical formula of molybdenum sulfide and tungsten sulfide of diisooctyl dithiophosphate is
R is isooctyl, i.e
X is S or O and the structural formula is as follows:
the inventionThe reaction process of the preparation method is as follows: (III)+ZDTP+R(COOH)2→ the product of the invention where H2S+NaOH→Na2Recycling of S and/or NaSH
DTP being a dialkyldithiophosphoric acid alkyl radical C5～C8
ZDTP is zinc dialkyldithiophosphate
The molybdenum sulfide tungsten sulfide (A) and zinc dialkyl dithiophosphate (B) have good synergistic effect, 150SN (C) is used as base oil, when A: B: C is 0.17: 0.33: 99.5, the friction-reducing and wear-resisting effects are optimal, a layer of film which is as bright as a mirror can be formed on the surface of a friction pair, and the oil sample temperature can be reduced by about 1 ℃ instead of being increased along with the extension of the friction time. The product of the present invention has good compatibility with lubricating oil of various brands, for example, on the basis of Kangrun 30QC, after the product of the present invention is added according to 1.5% (wt), and then the product is respectively added into an automobile engine, a gearbox and a main transmission, after an automobile runs for 500 kilometers, the oil saving rate when the automobile runs at constant speed of 30, 40, 50, 60 and 70Km/h is respectively 3.5%, 4.2%, 4.1%, 4.5% and 5.3%, namely the oil saving rate is correspondingly increased along with the increase of the automobile speed, which is the characteristic of the product of the present invention, and the characteristic is consistent with the development direction of machines, vehicles and ships to high speed, high load and high temperature operation conditions.
The product of the invention is brown liquid in appearance, the specific gravity is 1.08 +/-0.02, and the kinematic viscosity (40 ℃) is 94 +/-5 mm2And/s, the open flash point is 180 ℃, the condensation point is-17 ℃, the mechanical impurities are 0.014%, the acid value is 120 +/-5 KOHmg/g, and the result of a corrosion test at 120 ℃ for 3 hours is 1A, so that the qualified standard is reached. The product of the invention and base oil are mixed according to the proportion of 1: 4 and then added into 5W/30 CD-grade lubricating oil to carry out bearing capacity test (PB) under the condition of different addition amounts, which is shown in a table-3; the anti-sintering capability (PD) is shown in table-4, and when the product of the invention is added into engine oil by 3 percent, the PD value is increased by more than 50 percent, the anti-sintering load of the oil product is obviously improved, and the anti-sintering capability (PD) is prevented or improvedThe sintering and the damage of the machine are reduced,cylinder pulling and tile burning are prevented; the comprehensive wear index is shown in table-5, the comprehensive wear degree of an oil product is improved by more than 75% after 3% of the product is added, the wear resistance is obviously improved, the service life of a machine part is prolonged, the high-temperature wear resistance is shown in table-6, the wear degree can be obviously reduced by adding 3% of the product into the oil product, the diameter of a wear mark is reduced by 30%, and the service life of the machine part is prolonged; the antifriction property is shown in table-7, the friction coefficient is reduced by 29.79% by adding 3% of the product of the invention, the energy consumption (electricity consumption, oil consumption and the like) is reduced, and the friction-reducing agent has the energy-saving characteristic. The trial condition of the product user is shown in the table-8; the comparative data of the product of the invention and the like famous brand lubricating oil additives on the domestic and foreign markets are shown in the table-9; the raw materials used for preparing the invention are shown in the table-8, and the raw materials are all chemical products which are sold in the market.
The invention achieves the following effects:
(1) the preparation method of the invention adopts high-quality dialkyl dithiophosphoric acid as a raw material, thus solving the pollution problem in the production process;
(2) the product has no bad smell
(3) The product has good oil solubility, excellent friction reduction and wear resistance:
(A) the additive is added into base oil 150SN, 15W/40CD, wherein the molybdenum content is 100-300ppm, which can improve the PB value of a reference oil product by more than 135 percent; the friction coefficient mu value is reduced to 0.03-0.05.
(B) 0.5% of the additive of the invention is added into the base oil 150SN, and the temperature of the oil sample is not increased but decreased by about 1 ℃ along with the extension of the friction movement.
(4) The additive of the invention has wide application, can be added into various lubricating oils, can also be added into various prepared lubricating oils, can be used on operating equipment such as vehicles and ships, mining machinery, power generation equipment, metallurgy, machine tools, drilling and oil extraction and the like, and can achieve the functions of saving energy, reducing consumption, reducing cost and improving economic benefit.
Example 1
35 parts of molybdenum trioxide, 2 parts of tungsten trioxide and 8 parts of sodium hydroxide are added into a reactor (1) filled with a proper amount of water and stirred and mixed, at the temperature of about 45 ℃ under normal pressure for about 1 hour, then 4 parts of sodium sulfide is added to be continuously stirred and mixed for about 1 hour, the generated mixture of sodium molybdate sulfide and sodium tungstate sulfide enters a second reactor (2), and 10 parts of base oil, 12 parts of sulfuric acid, and 200 parts of diisooctyl dithiophosphoric acid are added into the reactor, simultaneously introducing nitrogen into the reactor (2) to protect the reaction, wherein the reaction temperature is about 100 ℃ and the reaction time is about 4 hours, cooling, washing for 3-4 times, heating to 100 deg.C for dewatering, the product of the invention can be prepared by adding 600ppm of unsaturated succinic acid, mixing and filtering, wherein the molybdenum content of the product is 9.0 percent, the tungsten content is 10000ppm, and the unsaturated succinic acid content is 600 ppm.
10 parts of the product is added into 1000 parts of lubricating oil base oil, the PB value is improved to 100Kg from the original 40Kg, and the friction coefficient is reduced to 0.092 from the original 0.260 Kg.
The product is added into 30QC engine oil by 1.5 percent (wt) and is tested on a Beijing 130 vehicle, the oil saving rates of urban areas, urban areas and express lane running modes are respectively 4.0 percent, 4.2 percent and 5.3 percent, and the contents of carbon monoxide and alkanes in automobile emission pollutants are respectively reduced by 11.1 percent and 16.7 percent.
The extreme pressure value of the product is increased from 509.6N which is not added with the additive to 1078.0N when the product is added into 5W/30CD by 0.5 percent (wt), the comprehensive wear index is improved by over 75 percent, the anti-wear performance is improved by 30 percent, and the anti-friction performance is improved by 29.79 percent.
Example 2
The procedure for the preparation of the lubricating oil additive is the same as in example 1, with the following raw material additions: the lubricating oil additive prepared from 25 parts of molybdenum trioxide, 1 part of tungsten trioxide, 4 parts of sodium hydroxide, 1 part of sodium sulfide, 140 parts of diisooctyl dithiophosphoric acid, 2 parts of hydrochloric acid, 3 parts of base oil, 700 parts of zinc dialkyl dithiophosphate and 5ppm of unsaturated succinic acid contains 1.0% of molybdenum, 700ppm of tungsten, 6.5% of zinc and 5ppm of unsaturated succinic acid.
Example 3
The procedure for the preparation of the lubricating oil additive is the same as in example 1, with the following raw material additions: 30 parts of molybdenum trioxide, 2 parts of tungsten trioxide, 2 parts of sodium hydroxide, 2.5 parts of sodium sulfide, 170 parts of diisooctyl dithiophosphate, 2 parts of acetic acid and 1 part of base oil are reacted, 5ppm of unsaturated succinic acid and 340 parts of ZDTP are added into a liquid product obtained by the reaction for blending to obtain the product, wherein the molybdenum content is 2.5%, the tungsten content is 6000ppm, the zinc content is 5.2% and the unsaturated succinic acid content is 5 ppm.
TABLE-1
| Name of raw materials | Standard of merit |
| Molybdenum trioxide | Industrial grade |
| Tungsten trioxide | Industrial grade |
| Sodium hydroxide | Chemical purity |
| Sodium sulfide | Chemical purity |
| Diisooctyl dithiophosphoric acid | Industrial grade |
| Base oil 150SN | Industrial grade |
| Zinc dialkyl dithiophosphate | Industrial grade |
| Unsaturated succinic acid | Chemical purity |
| Water (W) | |
| Sulfuric acid/hydrochloric acid/acetic acid | |
| H2SO4/HOR HAC | Chemical purity |
The raw materials are all market-friendly chemical products
The product is blended with a certain amount of lubricating oil base oil (150SN) to ensure MoThe content is about 0.5%, and the following comparative tests are carried out according to different proportions of the lubricating oil added into 5W/30 CD.
(1) Oil film bearing capacity
(2) Resistance to sintering load
(3) Composite wear index
(4) High temperature wear resistance
(5) Antifriction property
Wherein the reference oil physical property parameters are shown in the followingtable 2
5W/30CD table-2
(oil sample: 5W/30CD + formulated product) the specific test results are given in the following table. Load capacity test table-3
Anti-sintering capability test Table-4
Comprehensive wear index Table-5
| Item | Properties of |
| Kinematic viscosity 100 ℃ mm2/s | 10.80 |
| Flash point open DEG C | 202 |
| Pour point C | ＜-40 |
| Low temperature dynamic viscosity-25 deg.C MPa.S | 3500 |
| Sulfur content% | 0.23 |
| Content of phosphorus% | 0.073 |
| The addition amount of the blended product is% | PB.N | Improving ability% |
| 0 | 509.6 | 1 |
| 1.0 | 833.0 | 63.46 |
| 3.0 | 1078.0 | 111.54 |
| 5.0 | 1176.0 | 130.77 |
| 7.0 | 1372.0 | 169.23 |
| The addition amount of the prepared product is% | PD.N | Improving ability% |
| 0 | 1960.0 | 1 |
| 1.0 | 2450.0 | 25 |
| 3.0 | 3087.0 | 57.50 |
| 5.0 | 3087.0 | 57.50 |
| 7.0 | 3087.0 | 57.50 |
| The addition amount of the prepared product is% | ZMZ.N | Improving ability |
| 0 | 281.3 | 1 |
| 1.0 | 380.2 | 35.16 |
| 3.0 | 494.9 | 75.93 |
| 5.0 | 515.9 | 83.40 |
| 7.0 | 604.7 | 114.97 |
Abrasion resistance test Table-6
Antifriction Property test Table-7
Comparison of the carrying capacity of the product of the invention with that of the domestic and foreign additives Table 8
| The addition amount of the blended product is% | Abrasion spot diameter mm | Improving ability% |
| 0 | 0.40 | 1 |
| 1.0 | 0.36 | 10.00 |
| 3.0 | 0.28 | 30.00 |
| 5.0 | 0.30 | 25.00 |
| 7.0 | 0.30 | 25.00 |
| The addition amount of the blended product is% | Coefficient of friction | Improving ability |
| 0 | 0.094 | 1 |
| 1.0 | 1 | 1 |
| 3.0 | 0.066 | 29.79 |
| 5.0 | 0.087 | 7.45 |
| 7.0 | 0.031 | 67.02 |
| Numbering | Reference base oil | Kind of additive | Manufacturer of the product | The dosage of the additive is% | P8 Kg |
| 01 | 150SN | / | / | / | 40 |
| 02 | 150SN | Wanlingba | Canada | 2 | 54 |
| 03 | 150SN | The product (1) | / | 0.5 | 94 |
| 04 | 150SN | The product (2) | / | 5 | 100 |
| 05 | 30QC | / | / | / | 48 |
| 06 | 30QC | Peculiar smell | United states of America | 5 | 66 |
| 07 | 30QC | Comte of earl | United states of America | 5 | 114 |
| 08 | 30QC | Multiple force | Canada | 5 | 76 |
| 09 | 30QC | Wan Ji Ling (3) | Zhongxi Zhongshan | 2 | 126 |
| 10 | 5W/30CD | 0 | / | / | 51.9 |
| 11 | 5W/30CD | The product (2) | / | 1 | 84.9 |
| 12 | 5W/30CD | The product (2) | / | 3 | 109.9 |
| 13 | 5W/30CD | The product (2) | / | 5 | 119.9 |
| 14 | 5W/30CD | The product (2) | / | 7 | 139.9 |
User trial table-9
| Trial unit | Vehicle model | Oil saving rate | Tail gas | Feeling of activation | Noise(s) | Condition of engine oil | Remarks for note |
| Daxing county Transport bureau Department of transportation | Liberation 141 | 13.64％ | Is normal | Is normal | Low iron content | ||
| Yellow river 362 | 10.53％ | Improvement of life | Is normal | Is normal | Low iron content | ||
| Dongfeng 140 | 8.82％ | Improvement of life | Is normal | Is normal | Low iron content | ||
| Xingtong steam Taxi renting device Company(s) | Jilin | 2.80％ | Improvement of life | Good start | Descend | ||
| Xiali | 10％ | Descend | Improvement of life | Engine light Show improvement | |||
| Changhe 1010 | 2.86％ | Improvement of life | Good start | Descend | |||
| Stable pesticide Machine pipe Reason station | Oriental red-802 | 9.57％ | Improvement of life | Is converted to normal | Save for 47.9％ | ||
| Ox-55 | 8％ | Save for 8.33％ | |||||
| Ox-55 | 8.70％ | Save for 2.5％ | |||||
| Changzi camp and village Intermodal station | Oriental red 60 | 2.86％ | Starting is fast | ||||
| Beijing Bureau of public road Great office | Taituola | 8.05％ |
Claims (1)
1. A lubricating oil additive characterized by:
(1) putting 25-35 parts of molybdenum trioxide and 4-8 parts of sodium hydroxide into a reactor (1) filled with a proper amount of water, continuously stirring for 0.5-1.5 hours at normal temperature and normal pressure to generate sodium molybdate, adding 1-4 parts of tungsten trioxide, and continuously reacting for 0.5-1.0 hour to generate sodium tungstate;
(2) or adding 1-4 parts of sodium sulfide or sodium hydrosulfide into the reactor (1) to react with sodium molybdate and sodium tungstate to generate a mixture of sodium molybdate sulfide and sodium tungstate sulfide;
(3) putting the mixture of sodium molybdate sulfide and sodium tungstate sulfide in the reactor (1) into the reactor (2), adding 140-200 parts of diisooctyl dithiophosphoric acid, adding 2-12 parts of sulfuric acid or hydrochloric acid or acetic acid, introducing nitrogen, adding 3-10 parts of lubricating oil base oil 150SN, reacting at 80-100 ℃ for 3-5 hours to obtain a liquid product and discharging a small amount of hydrogen sulfide gas;
(4) washing the liquid product with water, settling, separating, crystallizing and filtering to obtain sulfurized diisooctyl zinc dithiophosphate (B), wherein the adding amount of the sulfurized diisooctyl zinc dithiophosphate (B) is that A to B is 0 to 5.0, and 5 to 600ppm of unsaturated succinic acid is added for blending to prepare the lubricating oil additive of the invention;
(5) the released hydrogen sulfide gas is absorbed by sodium hydroxide, and sodium sulfide or sodium hydrosulfide obtained after refining enters a reactor (1) for recycling;
(6) the lubricant additive contains main elements which account for 1.0-9.0 percent of molybdenum, 10000ppm of tungsten, 0-6.5 percent of zinc and 5-600ppm of unsaturated succinic acid in percentage by weight of the additive;
(7) the appearance of the lubricating oil additive is brown liquid, the specific gravity is 1.08 +/-0.02, and the lubricating oil additive is transportedThe dynamic viscosity (40 ℃) is 94 +/-5 mm2And/s, the open flash point is 180 ℃, the condensation point is-17 ℃, the mechanical impurities are 0.014 percent, and the acid value is 120 +/-5 KOHmg/g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96104720A CN1037520C (en) | 1996-04-23 | 1996-04-23 | Additive for lubricating oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96104720A CN1037520C (en) | 1996-04-23 | 1996-04-23 | Additive for lubricating oil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1138086A true CN1138086A (en) | 1996-12-18 |
| CN1037520C CN1037520C (en) | 1998-02-25 |
Family
ID=5118478
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96104720A Expired - Fee Related CN1037520C (en) | 1996-04-23 | 1996-04-23 | Additive for lubricating oil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1037520C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1315998C (en) * | 2002-04-05 | 2007-05-16 | 英菲诺姆国际有限公司 | Lubricating oil composition |
| CN100345949C (en) * | 2006-02-21 | 2007-10-31 | 刘洪良 | Prepn process of graphite/organic molybdenum lubricant oil prepn |
| CN111638151A (en) * | 2020-07-15 | 2020-09-08 | 一汽解放汽车有限公司 | Test method for detecting abrasion resistance of friction pair |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6187690A (en) * | 1984-10-05 | 1986-05-06 | Asahi Denka Kogyo Kk | Dialkylphosphorodithionic acid oxymolybdenum sulfide |
| NL8900362A (en) * | 1989-02-15 | 1990-09-03 | Philips Nv | METHOD AND APPARATUS FOR REGISTERING AND READING A MAGNETO-OPTICAL REGISTRATION CARRIER. |
| JP2642204B2 (en) * | 1989-12-14 | 1997-08-20 | シャープ株式会社 | Drive circuit for liquid crystal display |
| CN1037696C (en) * | 1992-01-18 | 1998-03-11 | 广西万机灵高新科技产业集团公司 | Lubricating oil containing organic tungsten and molybdenum additive |
-
1996
- 1996-04-23 CN CN96104720A patent/CN1037520C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1315998C (en) * | 2002-04-05 | 2007-05-16 | 英菲诺姆国际有限公司 | Lubricating oil composition |
| CN100345949C (en) * | 2006-02-21 | 2007-10-31 | 刘洪良 | Prepn process of graphite/organic molybdenum lubricant oil prepn |
| CN111638151A (en) * | 2020-07-15 | 2020-09-08 | 一汽解放汽车有限公司 | Test method for detecting abrasion resistance of friction pair |
| CN111638151B (en) * | 2020-07-15 | 2022-02-22 | 一汽解放汽车有限公司 | Test method for detecting abrasion resistance of friction pair |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1037520C (en) | 1998-02-25 |
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