CN1335320A - Synthesis of diisooctyl molybdenum dithiophosphate - Google Patents
Synthesis of diisooctyl molybdenum dithiophosphate Download PDFInfo
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- CN1335320A CN1335320A CN 00121857 CN00121857A CN1335320A CN 1335320 A CN1335320 A CN 1335320A CN 00121857 CN00121857 CN 00121857 CN 00121857 A CN00121857 A CN 00121857A CN 1335320 A CN1335320 A CN 1335320A
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Abstract
The synthesis of diisooctyl molybdenum dithiophosphate is an unique one of direct reaction of molyadate and thiophosphoric acid in the ion exchange resin as catalyst. The break-in oil with diisooctyl molybdenum dithiophosphate as main component has excellent break-in effect.
Description
The present invention relates to a kind of lubricating oil additive preparation method, especially a kind of molybdenum diisooctyl dithiophosphate preparation method belongs to the lubricating oil field.
As everyone knows, iC
8-MoDTP is a kind of lubricating oil additive with good antiwear and friction reduction property and energy-saving effect.A large amount of laboratories and road test show, the coefficient 50% or more of generally can reducing friction, and the most literature report can save energy 2～5%, and in addition, the sulphur molybdenum phosphate also has antioxygen and extreme pressure property preferably, is a kind of additive of multiple-effect energy.
The development and the production of molybdenum salt start from the sixties.People such as nineteen sixty-five Rowan.Engene.v have successfully synthesized six kinds of dialkyl group (aryl) molybdenum dithiophosphate, and after several years, R.T.Vanderbilt company begins the soluble organic molybdenum that produces oil.Commodity MOLYVANA by name and MOLYVANL.But after putting goods on the market, it does not obtain much attention, the only hundreds of tons of annual turnover.
The eighties, along with developing rapidly of automotive industry, organic molybdenum is subjected to extensive attention as friction improving agent, anti-wear agent, extreme pressure agent.RT VANDERBILT company fine oil-soluble organo-molybdenum compound not only is on sale throughout the U.S. and is also exported Japan and West Europe.After several years, the rising sun of Japan electrification worker Co., Ltd. has also released five kinds of oil soluble molybdenum dialkyl-dithiophosphate compounds, サ Network テ Ha-300, サ Network テ Ha-500, サ Network テ Ha-600 and サ Network テ Ha-474.
The development of molybdenum in China salt is started late in exploitation.The eighties, dibutyl (diethylhexyl) molybdenum dithiophosphates that also released one after another such as the positive chemical plant, footpath, Wuhan of China, ten thousand clever High-Tech. Group, T471 organic-molybdenum zinc recombiner, products such as T472 oil-soluble organic molybdenum tungsten recombiner and T473 sulphur phosphorus type molybdenum tungsten recombiner.
The method for preparing molybdenum diisooctyl dithiophosphate has multiple, concludes to get up can be divided into two classes: directly molybdenum method and reduction method.
Reduction method is in the process of sulphur phosphoric acid and the reaction of molybdenum source compound, adds reductive agent, as SO
2Deng; Perhaps before reaction, the sexavalence molybdenum is reduced to tetravalence, again with the sulphur phosphatase reaction.Adopt the synthetic iC of reduction method
8The document of-MoDTP is more, and for example, 1994 the 4th phases " lubricating oil " magazine is delivered by Wang Renfang work " reduction method is synthesized phosphorodithioic acid sulphur oxygen molybdenum ".Directly the molybdenum method is with sulphur phosphoric acid and the reaction of sexavalence molybdenum source compound.Traditional molybdenum diisooctyl dithiophosphate direct method preparation process comprises: six steps such as salify, acidifying, reaction, branch water, washing, distillation.The report of employing direct method has people's such as Sabol, Albert R United States Patent (USP) 956281 (1978); Li Yongde work " the synthetic and antifriction performance research of phosphorodithioic acid O, O-dialkyl-molybdenum compound moral " (1991).The preparation route as shown in Figure 1.
Traditional iC
8-MoDTP prepares not only route complexity, operational difficulty, quality less stable, and easily produces materials such as waste gas, waste water, and environment is caused great pollution.
The object of the invention is to provide a kind of molybdenum diisooctyl dithiophosphate and unique catalysis method preparation technology thereof of superior performance.The novel ion exchange resin of this process using is catalyzer, does not have strong acid and strong base to add in the reaction process.The present invention prepares route as shown in Figure 2.
The present invention is a catalyzer with ion exchange resin, adopts the non-alkali direct method of non-acid technology, has obtained forming the iC that is different from traditional technology
8-MoDTP product has not only reduced production cost significantly, has simplified synthesis step, and pollution is alleviated, and environment protection and health of human body are had positive effect.
IC of the present invention
8-MoDTP preparation method is as follows: add 80～120 parts of thiophosphoric anhydrides, 40.5～44.5 parts of isooctyl alcohol in there-necked flask, stir down at 75～90 ℃ and made sulphur phosphoric acid in 3.0～6.0 hours.The ion exchange resin that adds 34～48 parts of molybdates and 2～6 parts again, the sherwood oil that after reacting 5.0～7.0 hours under 80.0～90.0 ℃, adds 180～220 parts 90～120 ℃, reactant leave standstill be divided into immediately in 5～10 minutes two-layer, branch vibration layer and catalyzer.Promptly obtain the molybdenum diisooctyl dithiophosphate product after steaming solvent.
With present method synthetic iC
8-MoDTP is that the running in oil that the host mediation forms is united evaluation through Shanghai Communications University, Shanghai Tractor Internal Combustion Engine Co., proves that its performance is very superior.Use this running in oil every that Shanghai Tractor Internal Combustion Engine Co. produces can be reduced 25 minutes at sold inside the country machine seating time, every export trade machine seating time reduces 60 minutes.
The present invention has two width of cloth accompanying drawings, and Fig. 1 is synthetic iC
8-MoDTP tradition direct method operational path.Fig. 2 is this bright iC
8-MoDTP prepares route.
Following embodiment further specifies of the present invention, rather than limits the invention.Spirit of the present invention and protection domain are listed in claims.
Embodiment 1: add isooctyl alcohol 80.0 grams in there-necked flask, thiophosphoric anhydride 40.5 grams are warming up to 75 ℃ and stirred 3.0 hours.Obtain sulphur phosphatase 11 10.0 grams.Add ammonium molybdate 34.0 gram, ion exchange resin 2.0 grams again, be warming up to 80.0 ℃, react and add sherwood oil 180.0 after 5.0 hours and restrain, stir 10 minutes, leave standstill after 5 minutes and obtain layering solution.Branch vibration layer and be deposited in the catalyzer of container bottom, steaming desolventizes, and obtains iC
8-MoDTP product 136.0 grams.Its analytical data is as follows: Mo content 9.5%, S content 14.2%, P content 7.3%, acid number 122mgKOH/g, 146.0 ℃ of flash-points, the iC with 4 ‰
8-MoDTP adds 9
#Low-grade fever stirs and was mixed into running in oil in 10 minutes in the oil, and its analytical data is as follows: mill spot area 0.5mm
2, P
B: 980N, P
D: 1960N, copper corrosion: 1b.
Embodiment 2: add isooctyl alcohol 100.0 grams in there-necked flask, thiophosphoric anhydride 42.5 grams are warming up to 85 ℃ and stirred 4.0 hours, obtain sulphur phosphatase 11 40.0 grams.Add Sodium orthomolybdate 48.0 grams again, ion exchange resin 4.0 grams are warming up to 85.0 ℃ of reactions 5.0 hours.Reaction finishes the back and divides the water intaking layer, and steaming desolventizes, and obtains iC
8-MoDTP product 176.0 grams.Its analytical data is as follows: Mo content 8.7%, S content 15.82%, P content 6.7%, acid number 108mgKOH/g, 124 ℃ of flash-points, the iC with 4 ‰
8-MoDTP adds 9
#Low-grade fever stirs and was mixed into running in oil in 10 minutes in the oil, and its analytical data is as follows: mill spot area 0.48mm
2, P
B: 883N, P
D: 1568N, copper corrosion: 1b.
Embodiment 3: add isooctyl alcohol 120.0 grams in there-necked flask, thiophosphoric anhydride 44.5 grams are warming up to 85 ℃ and stirred 6.0 hours, obtain sulphur phosphatase 11 60.0 grams.Add ammonium molybdate 34.0 grams again, ion exchange resin 6.0 grams are warming up to 90.0 ℃, react to add sherwood oil 220.0 grams after 7.0 hours, stir 10 minutes, leave standstill after 5 minutes and obtain layering solution.Branch vibration layer and be deposited in the catalyzer of container bottom, steaming desolventizes, and obtains iC
8-MoDTP product 183.0 grams.Its analytical data is as follows: Mo content 9.1%, S content 15.39%, P content 6.76%, acid number 116mgKOH/g, 134 ℃ of flash-points, the iC with 4 ‰
8-MoDTP adds 9
#Low-grade fever stirs and was mixed into running in oil in 10 minutes in the oil, and its analytical data is as follows: mill spot area 0.5mm
2, P
B: 1029.ON, P
D: 1960N, copper corrosion: 2b.
Claims (3)
1. molybdenum diisooctyl dithiophosphate and preparation method thereof, it is characterized in that: thiophosphoric anhydride and isooctyl alcohol stir down at 85 ℃ and made sulphur phosphoric acid in 4 hours, again with a certain amount of molybdate at ion-exchange resin catalyst, react after 5～7 hours, the sherwood oil that adds 90～120 ℃, reactant leave standstill and were divided into two-layerly in 5 minutes immediately, divide to remove moisture and catalyzer, steaming desolventizes, and promptly obtains the molybdenum diisooctyl dithiophosphate product.
2. method according to claim 1, it is characterized in that: each reacts the component consumption and is respectively 80～100 parts of thiophosphoric anhydrides, 40.5～44.5 parts of isooctyl alcohol, the ion exchange resin of 34～48 parts of molybdates and 2～6 parts, 180～220 parts 90～120 ℃ sherwood oil obtains 136～183 parts of molybdenum diisooctyl dithiophosphates.
3. method according to claim 1 is characterized in that: the iC of preparation
8-MoDTP can be applied in running in oil, gear oil, the vehicle transmission wet goods technical oils.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 00121857 CN1335320A (en) | 2000-07-25 | 2000-07-25 | Synthesis of diisooctyl molybdenum dithiophosphate |
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| CN 00121857 CN1335320A (en) | 2000-07-25 | 2000-07-25 | Synthesis of diisooctyl molybdenum dithiophosphate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980320A (en) * | 2014-05-16 | 2014-08-13 | 中国石油大学(华东) | Oil soluble molybdenum-based precursor of catalyst, preparation method and application thereof |
| CN107312031A (en) * | 2017-06-22 | 2017-11-03 | 新乡市瑞丰新材料股份有限公司 | A kind of preparation method of di-isooctyl dithio zinc phosphate salt |
| EP3581635A1 (en) | 2018-06-16 | 2019-12-18 | INDIAN OIL CORPORATION Ltd. | Hydrocarbon soluble metal compositions and method of making them |
-
2000
- 2000-07-25 CN CN 00121857 patent/CN1335320A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980320A (en) * | 2014-05-16 | 2014-08-13 | 中国石油大学(华东) | Oil soluble molybdenum-based precursor of catalyst, preparation method and application thereof |
| CN107312031A (en) * | 2017-06-22 | 2017-11-03 | 新乡市瑞丰新材料股份有限公司 | A kind of preparation method of di-isooctyl dithio zinc phosphate salt |
| EP3581635A1 (en) | 2018-06-16 | 2019-12-18 | INDIAN OIL CORPORATION Ltd. | Hydrocarbon soluble metal compositions and method of making them |
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