CN102776054B - Preparation method of viscosity index improver with high shear resistance - Google Patents
Preparation method of viscosity index improver with high shear resistance Download PDFInfo
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- CN102776054B CN102776054B CN201110124569.5A CN201110124569A CN102776054B CN 102776054 B CN102776054 B CN 102776054B CN 201110124569 A CN201110124569 A CN 201110124569A CN 102776054 B CN102776054 B CN 102776054B
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Abstract
The invention discloses a preparation method of a viscosity index improver with high shear resistance for lubricating oil. The method mainly conducts exploratory research on production technologies of an ethylene-propylene copolymer viscosity index improver, makes use of an accelerator, combines an integrated process of mechanical degradation, thermal degradation and oxidation degradation, effectively controls the product quality, and fully enhances the shear resistance of the product. The product comprises, by mass: 10-20% of the ethylene-propylene copolymer, 0.05-6% of the accelerator, and the balance base oil. The product has a thickening ability of 3.0-8.0mm<2>.s<-1>, a diesel nozzle shear stability index SSI (100DEG C) of 0-20. And the product can be widely used in high-grade internal combustion engine oil, hydraulic oil, and gear oil products. The technology disclosed in the invention has the advantages of simple operation, mild condition, and environmental friendliness.
Description
(1) technical field
The present invention relates to a kind of preparation method of high anti-shear performance viscosity index improver.This product can be widely used in, in high-grade I. C. engine oil, hydraulic efficiency oil and gear oil product, belonging to lubricating oil field.
(2) background technology
The development of automobile industry, has proposed more and more higher requirement to automobile oil.In order to meet the harsh operating conditions such as high speed, high loading, low temperature, the basic researchs such as the use properties to the various Additive Properties that add in lubricating oil, additive evaluation means and additive product have proposed more and more higher requirement.Along with the continuous renewal of engine and the requirement economizing on resources, I. C. engine oil is fast to superior and future development multi-grade oil.In the time of development multi-grade oil, in order to meet the high and low temperature performance of oil product, need in used more low viscous base oil, add oil soluble chain high molecular polymer, i.e. viscosity index improver, is also tackifier.Be mainly used in I. C. engine oil, hydraulic efficiency oil, automatic transmission fluid and gear oil.Viscosity index improver can not only multiviscosisty base oil, improves the viscosity temperature characteristic of oil product, makes oil product have good high temperature lubricating and low-temperature fluidity, and can reduce the consumption of fuel and lubricating oil, realizes oil product universalization.In the time of modulation multi-grade oil, generally all can add the viscosity index improver of 4%-9% left and right, its consumption accounts for 22% left and right of oil dope total amount.
Conventional viscosity index improver has polymethacrylate (PMA), polyisobutene (PIB), ethylene-propylene copolymer (OCP), hy drogenated styrene-diene copolymer (HSD), vinylbenzene polyester and poly-n-butyl vinyl ether (BB) etc.Although various types of viscosity index improvers all have the effect that improves oil product viscosity temperature characteristic, its thickening capabilities, shear stability, thermal oxidation stability, low-temperature performance and economy but have larger difference.In many viscosity index improver products, the feature such as OCP type viscosity index improver has tackifying ability and shear stability is better, high-temperature behavior is good and on-the-spot use properties is good, price is also moderate, is a kind of using in the world morely at present.OCP is used widely in I. C. engine oil, and particularly diesel engine oil, in the consumption of viscosity index of internal combustion engine oil improving agent, accounts for more than 80%.It is a class of current consumption maximum.Since releasing first OCP viscosity index improver the seventies, this product has obtained and has developed rapidly, and sales volume has accounted for the more than 60% of whole viscosity index improver (VII).According to statistics, within 2008, China's oil production is about 6,400,000 tons, approximately 60,000 tons of left and right of all kinds of viscosity index improver demands.Within 2009, China's oil production is about 7,400,000 tons, and all kinds of viscosity index improver demands are about 70,000 tons.Can calculate, wherein the demand of OCP viscosity index improver should be more than 40,000 tons, and market outlook are boundless.For the large feature of viscosity index improver consumption, as Mobil, Exxon, Rohm-hass etc., all the production to viscosity index improver and development are paid much attention in global Ge great lubricant corporation.
The at present work of the good OCP type viscosity index improver of nature of production mainly concentrates on two aspects:
Be directly synthetic on the one hand, strictly control polymericular weight.
The experimentation of second the third polymerization comprises distribution, polymerization, flash distillation, denitrating catalyst, cohesion, extruding drying and other steps.First the ethene of polymerization-grade, propylene and hydrogen is respectively through super-dry (ethene also passes through deoxidation), after metering through two sections of compressions, be condensed into liquid, enter in mix monomer tank, for polymerization charge.When polymerization, raw material and the catalyzer that configures and anti-aging agent, activator are joined in polymeric kettle, at certain pressure, temperature, obtain polymerization glue through the reaction of certain hour.This glue obtains finished product after the aftertreatments such as above-mentioned flash distillation.
Be by second higher molecular weight the third glue on the other hand, arrive certain molecular weight by thermooxidizing or mechano-degradation.Commercially available second the third glue is mainly for example, from some external major companies: Mobil, Du Pont, Dutch DSM, Mitsui chemistry etc., domestic only have Jilin Petrochemical to produce.At present, domestic each additive factory owner will adopt degradation technique to produce all kinds of OCP type viscosity index improvers, comparative maturity of its related process, but palliating degradation degree is difficult to control, and must after reaction finishes, add base oil and carry out secondary adjusting, certainly will cause the difference of different batches product inner quality, quality product is wayward, the shear stability of product is relatively poor, shears index (SSI) between diesel fuel nozzle all more than 20, in being used for, in low-grade I. C. engine oil product.Restrict to a great extent this type of viscosity index improver range of application and development prospect.
(3) summary of the invention
The invention provides a kind of preparation method of high anti-shear performance viscosity index improver.
The object of the invention is to provide a kind of preparation method of high anti-shear performance viscosity index improver.
Method provided by the invention comprises: add quantitative base oil to specifying in reactor, open reactor and stir, slowly add quantitative promotor from reactor top solid feed inlet, reactor is heated up.The temperature rise of question response still is to 40-80 DEG C, starts at the uniform velocity to add quantitative ethylene-propylene copolymer blob of viscose, after adding glue and adding, continues to be warming up to 120-200 DEG C, keeps temperature-stable, opens gas valve, to reactor blowing air, and reaction 1-10h.After reaction finishes, stop blowing air, cooling, termination reaction.The thickening ability of product is 3.0-8.0mm
2s
-1, diesel injector shear stability index SSI (100 DEG C) is 0-20.
Described promotor is one or more the composition in different carbon number alkylamines.Alkylamine carbon number is 4-48, is preferably 8-24, and more excellent is 18.Promotor add-on is 0.01-8wt%.Be preferably 0.05-6wt%.
Described ethylene-propylene copolymer is one or more composition of multiple binary ethylene propylene copolymer.Add-on is 10-20wt%, is preferably 12-18wt%.
Described base oil is high viscosity index (HVI) I class or II class high-quality base oil, and 100 DEG C of kinematic viscosity of base oil are 3-10mm
2/ s, is preferably 4-6mm
2/ s.Viscosity index is greater than 90.
Described air flow quantity refers to raw material per ton charge volume amount hourly, is 0.1m
3/ h ﹒ t～100m
3/ h ﹒ t, is preferably 1m
3/ h ﹒ t～80m
3/ h ﹒ t, more excellent is 10m
3/ h ﹒ t～50m
3/ h ﹒ t.
Feed temperature is 40-80 DEG C, is preferably 50-60 DEG C.
Temperature of reaction is 120-200 DEG C, is preferably 140-180 DEG C.
Duration of the reaction is 1-10 hour, and the reaction times is 2-8 hour preferably, and more excellent is 2-6 hour.
The high anti-shear performance viscosity index improver product that the inventive method makes, thickening ability is 3.0-8.0mm
2s
-1, diesel injector shear stability index SSI (100 DEG C) is 0-20.
The inventive method relates to that technological operation is simple, mild condition, environmental friendliness.The method is than current preparation method, can effectively improve the anti-shear performance of product, rationally regulate the relation of thickening capabilities and cutting performance, and can obtain the series product with different shear stability indexes by adjusting process parameter, range of application and the development prospect of greatly having expanded OCP type viscosity index improver, product can be widely used in high-grade I. C. engine oil, hydraulic efficiency oil and gear oil.
Below in conjunction with embodiment, the present invention is described in detail.
(4) embodiment
Embodiment 1
In the 200ml Glass Containers of being furnished with agitator, thermometer, heating jacket and air feed channel, add base oil 86g, open and stir, then add 0.05g stearylamine, be warming up to 50 DEG C, then second the third glue that adds 14g to be cut into small pieces.Stir, be warming up to 130 DEG C, react 4 hours, continue to be warming up to 160 DEG C, pass into air, flow 100ml/min, reacts 2 hours.After reaction finishes, stop ventilation, cooling discharge.Product carries out analytical test according to petrochemical complex SH/T0622-2007 standard.Its thickening ability is 3.3mm
2s
-1, diesel injector shear stability index SSI (100 DEG C) is 0.
Embodiment 2
In the 250ml Glass Containers of being furnished with agitator, thermometer, heating jacket and air feed channel, add base oil 127g, open and stir, then add 1g stearylamine, be warming up to 45 DEG C, then second the third glue that adds 22g to be cut into small pieces.Pass into air, flow 200ml/min, stirs, and is warming up to 130 DEG C, and the reaction times is 8 hours.After reaction finishes, stop ventilation, cooling discharge.Product carries out analytical test according to petrochemical complex SH/T0622-2007 standard.Its thickening ability is 3.6mm
2s
-1, diesel injector shear stability index SSI (100 DEG C) is 2.7.
Embodiment 3
In the 250ml Glass Containers of being furnished with agitator, thermometer, heating jacket and air feed channel, add base oil 127g, open and stir, then add 1g stearylamine, be warming up to 40 DEG C, then second the third glue that adds 22g to be cut into small pieces.Stir, be warming up to 130 DEG C, react 4 hours, continue to be warming up to 160 DEG C, pass into air, flow 200ml/min, reacts 4 hours.After reaction finishes, stop ventilation, cooling discharge.Product carries out analytical test according to petrochemical complex SH/T0622-2007 standard.Its thickening ability is 5.4mm
2s
-1, diesel injector shear stability index SSI (100 DEG C) is 16.1.
Embodiment 4
In the 1000ml Glass Containers of being furnished with agitator, thermometer, heating jacket and air feed channel, add base oil 680g, open and stir, then add 20g stearylamine, be warming up to 55 DEG C, then second the third glue that adds 120g to be cut into small pieces.Pass into air, flow 1000ml/min, stirs, and is warming up to 160 DEG C, reacts 3 hours.After reaction finishes, stop ventilation, cooling discharge.Product carries out analytical test according to petrochemical complex SH/T0622-2007 standard.Its thickening ability is 5.2mm
2s
-1, diesel injector shear stability index SSI (100 DEG C) is 8.0.
Embodiment 5
To the base oil that pumps into 85kg in 200L reactor, open reactor and stir, slowly add 0.5kg stearylamine from reactor top solid feed inlet, open steam reactor is heated up.The temperature rise to 80 DEG C of question response still, starts at the uniform velocity to add 20cm
3the second third adhesive tape 15kg of left and right size, after adding glue and adding, continues to be warming up to 140 DEG C, keeps temperature-stable, opens gas valve, to reactor blowing air, and flow 0.33m
3/ h, reaction 6h.After reaction finishes, stop blowing air, chuck water flowing is cooled to 80 DEG C of left and right, product discharge barrelling to reactor.Product carries out analytical test according to petrochemical complex SH/T0622-2007 standard.Its thickening ability is 6.2mm
2s
-1, diesel injector shear stability index SSI (100 DEG C) is 16.9.
Embodiment 6
To 10m
3in reactor, pump into 7000kg base oil, open reactor and stir, slowly add 40kg stearylamine from reactor top solid feed inlet, open steam reactor is heated up.The temperature rise to 40 DEG C of question response still, starts at the uniform velocity to add 1000cm
3the second third blob of viscose 1200kg of left and right size, after adding glue and adding, continues to be warming up to 140 DEG C, keeps temperature-stable, opens gas valve, to reactor blowing air, and flow 25m
3/ h, reaction 4h.After reaction finishes, stop blowing air, chuck water flowing is cooled to 80 DEG C of left and right, discharging to reactor.Product carries out analytical test according to petrochemical complex SH/T0622-2007 standard.Its thickening ability is 6.6mm
2s
-1, diesel injector shear stability index SSI (100 DEG C) is 15.0.
Claims (4)
1. the preparation method of a high anti-shear performance viscosity index improver, it is characterized in that: add quantitative base oil to specifying in reactor, unlatching reactor stirs, slowly add quantitative promotor from reactor top solid feed inlet, reactor is heated up, the temperature rise of question response still is to 40-80 DEG C, start at the uniform velocity to add quantitative ethylene-propylene copolymer blob of viscose, after adding glue, continue to be warming up to 120-200 DEG C, keep temperature-stable, open gas valve, to reactor blowing air, reaction 2-6h, after reaction finishes, stop blowing air, cooling, termination reaction, product discharge, in reaction, promotor used is that carbon number is 18 alkylamine, air flow quantity is 0.1m
3/ h ﹒ t～100m
3/ h ﹒ t, described material rate is: the content of ethylene-propylene copolymer is 10-20wt%, and accelerator content is 0.05-6wt%, and surplus is base oil.
2. the preparation method of a kind of high anti-shear performance viscosity index improver according to claim 1, is characterized in that: described ethylene-propylene copolymer is one or more the composition in multiple binary ethylene propylene copolymer.
3. the preparation method of a kind of high anti-shear performance viscosity index improver according to claim 1, is characterized in that: described base oil is high viscosity index (HVI) I class or II class base oil, and 100 DEG C of kinematic viscosity of base oil are 3-10mm
2/ s, viscosity index is greater than 90.
4. the preparation method of a kind of high anti-shear performance viscosity index improver according to claim 1, is characterized in that: described air flow quantity is 10m
3/ h ﹒ t～50m
3/ h ﹒ t.
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| CN104031195B (en) * | 2013-03-06 | 2016-10-12 | 中国石油天然气股份有限公司 | A kind of preparation method of viscosity index improver |
| WO2016200642A1 (en) | 2015-06-11 | 2016-12-15 | Bridgestone Americas Tire Operations, Llc | Rubber compositions containing viscosity modifier and related methods |
| CN110257137A (en) * | 2019-05-09 | 2019-09-20 | 泉州市欧美润滑油制品有限公司 | 120000 kilometers long oil draining period heavy duty automobile lubricating oil and preparation method thereof |
| CN114276857B (en) * | 2021-12-30 | 2023-07-04 | 金丰宏溢科技(佛山)有限公司 | OCP viscosity index improver |
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| US3756954A (en) * | 1971-09-16 | 1973-09-04 | Lubrizol Corp | Rs for lubricants degraded ethylene propylene interpolymers useful as viscosity modifie |
| US4068056A (en) * | 1975-03-05 | 1978-01-10 | Exxon Research And Engineering Company | Aminated polymeric additives for fuel and lubricants |
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