CN102776054A - 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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- CN102776054A CN102776054A CN2011101245695A CN201110124569A CN102776054A CN 102776054 A CN102776054 A CN 102776054A CN 2011101245695 A CN2011101245695 A CN 2011101245695A CN 201110124569 A CN201110124569 A CN 201110124569A CN 102776054 A CN102776054 A CN 102776054A
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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, 0.01-8% 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 belonging to the lubricating oil field in high-grade I. C. engine oil, hydraulicefficiency oil and the gear oil product.
(2) background technology
The development of automobile industry has proposed increasingly high requirement to automobile oil.In order to satisfy harsh operating conditions such as high speed, high loading, low temperature, increasingly high requirement has been proposed for the basic researchs such as use properties of the various additive performances, additive evaluation means and the additive product that add in the lubricating oil.Along with the continual renovation of mover and the requirement that economizes on resources, I. C. engine oil develops with direction multi-grade oil to superior fast.When the development multi-grade oil, in order to satisfy the high and low temperature performance of oil product, need in employed more low viscous base oil, add oil soluble chain high molecular polymer, promptly viscosity index improver also is tackifier.Be mainly used in I. C. engine oil, hydraulicefficiency oil, automatic transmission fluid and the gear oil.Viscosity index improver can not only the multiviscosisty base oil, improves the viscosity temperature characteristic of oil product, makes oil product have excellent high-temperature lubrication property and low-temperature fluidity, and can reduce the consumption of fuel and lubricating oil, realizes the oil product universalization.When the modulation multi-grade oil, generally all can add the viscosity index improver about 4%-9%, its consumption accounts for about 22% of oil dope total amount.
Viscosity index improver commonly used has Rohm tech inc (PMA), polyisobutene (PIB), ethylene-propylene copolymer (OCP), hydrogenated styrene diene copolymer (HSD), vinylbenzene polyester and gathers n-butyl vinyl ether (BB) etc.Though various types of viscosity index improvers all have the effect that improves the oil product viscosity temperature characteristic, its thickening capabilities, shear stability, thermal oxidation stability, low-temperature performance and economy but have bigger difference.In many viscosity index improver products, OCP type viscosity index improver has tackifying ability and shear stability is better, high-temperature behavior reaches characteristics such as on-the-spot use properties is good well, and price is also moderate, is a kind of using morely in the world 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 maximum one type of present consumption.Since releasing the OCP viscosity index improver first the seventies, this product has obtained to develop rapidly, and Absatzvolumen has accounted for more than 60% of whole viscosity index improver (VII).According to statistics, China's oil production was about 6,400,000 tons in 2008, about about 60,000 tons of all kinds of viscosity index improver demands.China's oil production was about 7,400,000 tons in 2009, and all kinds of viscosity index improver demands are about 70,000 tons.Can calculate that wherein the demand of OCP viscosity index improver should be more than 40,000 tons, market outlook are boundless.To the big characteristics of viscosity index improver consumption, each big lubricant corporation of the whole world such as Mobil, Exxon, Rohm-hass etc. pay much attention to the production and the development of viscosity index improver.
The work of the OCP type viscosity index improver that present nature of production is good mainly concentrates on two aspects:
Be directly synthetic on the one hand, strict controlling polymers molecular weight.
The second third polymeric experimentation comprises distribution, polymerization, flash distillation, denitrating catalyst, cohesion, extruding drying and other steps.At first the ethene of polymerization-grade, propylene and hydrogen is respectively through super-dry (ethene also passes through deoxidation), and metering gets in the mix monomer jar after two sections compressions, be condensed into liquid, supplies polymerization charge usefulness.During polymerization raw material and the catalyzer that configures and anti-aging agent, acvator are joined in the polymeric kettle, the reaction through certain hour under certain pressure, temperature obtains the polymerization glue.This glue obtains finished product after aftertreatments such as above-mentioned flash distillation.
Be second third glue that molecular weight is higher on the other hand, arrive certain molecular weight through thermooxidizing or mechano-degradation.Commercially available second third glue is mainly from some external major companies, for example: Mobil, Du Pont, Dutch DSM, Mitsui chemistry etc., domestic only have Jilin Petrochemical production.At present, domestic each additive factory owner will adopt degradation technique to produce all kinds of OCP type viscosity index improvers, and its related process is comparative maturity; But palliating degradation degree is difficult to control, must after reaction finishes, add base oil and carry out the 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 relatively, shears index (SSI) between diesel fuel nozzle all more than 20, in being used for, in the low-grade I. C. engine oil product more.Restricted this type of viscosity index improver range of application and development prospect to a great extent.
(3) summary of the invention
The invention provides a kind of preparation method of high anti-shear performance viscosity index improver.
The objective 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: in specifying reactor drum, add quantitative base oil, open reactor drum and stir, solid feed inlet slowly adds quantitative promotor from the reaction kettle top, and reactor drum is heated up.Question response still temperature rises to 40-80 ℃, and beginning at the uniform velocity adds quantitative ethylene-propylene copolymer blob of viscose, add glue add finish after, continue to be warming up to 120-200 ℃, keep temperature-stable, open gas valve, to the reactor drum blowing air, reaction 1-10h.Reaction stops blowing air after finishing, cooling, termination reaction.The thickening ability of product is 3.0-8.0mm
2S
-1, diesel fuel nozzle shear stability index SSI (100 ℃) is 0-20.
Described promotor is one or more the compsn in the different carbon number alkylamines.The alkylamine carbon number is 4-48, is preferably 8-24, and more excellent is 12-18.The promotor add-on is 0.01-8wt%.Be preferably 0.05-6wt%.
Described ethylene-propylene copolymer is one or more a compsn 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 ℃ 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 is meant 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 ℃, is preferably 50-60 ℃.
Temperature of reaction is 120-200 ℃, is preferably 140-180 ℃.
Duration of the reaction is 1-10 hour, and the reaction times is 2-8 hour preferably.
The high anti-shear performance viscosity index improver product that the inventive method makes, thickening ability is 3.0-8.0mm
2S
-1, diesel fuel nozzle shear stability index SSI (100 ℃) is 0-20.
The inventive method relates to that technological operation is simple, mild condition, environmental friendliness.This method is than present preparation method; Can effectively improve the anti-shear performance of product; Rationally regulate the relation of thickening capabilities and cutting performance; And can obtain to have the series product of different shear stability indexes through the adjusting process parameter, greatly expand the range of application and the development prospect of OCP type viscosity index improver, product can be widely used in high-grade I. C. engine oil, hydraulicefficiency oil and the gear oil.
Below in conjunction with embodiment, the present invention is specified.
(4) embodiment
Embodiment 1
In the 200ml Glass Containers of being furnished with whisking appliance, TM, heating jacket and air feed channel, add base oil 86g, open and stir, add the 0.05g stearylamine then, be warming up to 50 ℃, add second third glue that 14g is cut into small pieces again.Stir, be warming up to 130 ℃, reacted 4 hours, continue to be warming up to 160 ℃, bubbling air, flow 100ml/min reacted 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 fuel nozzle shear stability index SSI (100 ℃) is 0.
Embodiment 2
In the 250ml Glass Containers of being furnished with whisking appliance, TM, heating jacket and air feed channel, add base oil 127g, open and stir, add the 1g stearylamine then, be warming up to 45 ℃, add second third glue that 22g is cut into small pieces again.Bubbling air, flow 200ml/min stirs, and is warming up to 130 ℃, 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 fuel nozzle shear stability index SSI (100 ℃) is 2.7.
Embodiment 3
In the 250ml Glass Containers of being furnished with whisking appliance, TM, heating jacket and air feed channel, add base oil 127g, open and stir, add the 1g stearylamine then, be warming up to 40 ℃, add second third glue that 22g is cut into small pieces again.Stir, be warming up to 130 ℃, reacted 4 hours, continue to be warming up to 160 ℃, bubbling air, flow 200ml/min reacted 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 fuel nozzle shear stability index SSI (100 ℃) is 16.1.
Embodiment 4
In the 1000ml Glass Containers of being furnished with whisking appliance, TM, heating jacket and air feed channel, add base oil 680g, open and stir, add the 20g stearylamine then, be warming up to 55 ℃, add second third glue that 120g is cut into small pieces again.Bubbling air, flow 1000ml/min stirs, and is warming up to 160 ℃, 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 fuel nozzle shear stability index SSI (100 ℃) is 8.0.
Embodiment 5
In the 200L reaction kettle, pump into the base oil of 85kg, open reaction kettle and stir, solid feed inlet slowly adds the 0.5kg stearylamine from the reaction kettle top, opens steam reaction kettle is heated up.Question response still temperature rises to 80 ℃, and beginning at the uniform velocity adds 20cm
3About the second third adhesive tape 15kg of size, add glue add finish after, continue to be warming up to 140 ℃, keep temperature-stable, open gas valve, to the reaction kettle blowing air, flow 0.33m
3/ h, reaction 6h.Reaction stops blowing air after finishing, and the chuck water flowing is cooled to about 80 ℃ reaction kettle, product discharging barrelling.Product carries out analytical test according to petrochemical complex SH/T0622-2007 standard.Its thickening ability is 6.2mm
2S
-1, diesel fuel nozzle shear stability index SSI (100 ℃) is 16.9.
Embodiment 6
To 10m
3Pump into the 7000kg base oil in the reaction kettle, open reaction kettle and stir, solid feed inlet slowly adds the 40kg stearylamine from the reaction kettle top, opens steam reaction kettle is heated up.Question response still temperature rises to 40 ℃, and beginning at the uniform velocity adds 1000cm
3About the second third blob of viscose 1200kg of size, add glue add finish after, continue to be warming up to 140 ℃, keep temperature-stable, open gas valve, to the reaction kettle blowing air, flow 25m
3/ h, reaction 4h.Reaction stops blowing air after finishing, and the chuck water flowing is cooled to about 80 ℃ reaction kettle, discharging.Product carries out analytical test according to petrochemical complex SH/T0622-2007 standard.Its thickening ability is 6.6mm
2S
-1, diesel fuel nozzle shear stability index SSI (100 ℃) is 15.0.
Claims (8)
1. the preparation method of a high anti-shear performance viscosity index improver is characterized in that: in the appointment reactor drum, add quantitative base oil, open reactor drum and stir, the quantitative promotor of the slow adding of solid feed inlet from the reaction kettle top; Reactor drum is heated up, and question response still temperature rises to 40-80 ℃, and beginning at the uniform velocity adds quantitative ethylene-propylene copolymer blob of viscose, after adding glue and finishing; Continue to be warming up to 120-200 ℃, keep temperature-stable, open gas valve, to the reactor drum blowing air; Reaction 1-10h, reaction stops blowing air after finishing; Cooling, termination reaction, product discharging.
2. the preparation method of a kind of high anti-shear performance viscosity index improver according to claim 1 is characterized in that: described material rate is: the content of ethylene-propylene copolymer is 10-20wt%, and accelerator content is 0.01-8wt%, and surplus is a base oil.
3. the preparation method of a kind of high anti-shear performance viscosity index improver according to claim 1 is characterized in that: described promotor is that carbon number is one or more the compsn in the alkylamine of 4-48.
4. 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 compsn in the multiple binary ethylene propylene copolymer.
5. 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 ℃ of kinematic viscosity of base oil are 3-10mm
2/ s, viscosity index is greater than 90.
6. 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 0.1m
3/ h.t～100m
3/ h.t.
7. the preparation method of a kind of high anti-shear performance viscosity index improver according to claim 3 is characterized in that: described promotor is that carbon number is one or more the compsn in the alkylamine of 8-24.
8. the preparation method of a kind of high anti-shear performance viscosity index improver according to claim 6 is characterized in that: described air flow quantity is 10m
3/ h.t～50m
3/ h.t.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031195A (en) * | 2013-03-06 | 2014-09-10 | 中国石油天然气股份有限公司 | Preparation method for viscosity index improver |
| 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 |
| US10479881B2 (en) | 2015-06-11 | 2019-11-19 | Bridgestone Americas Tire Operations, Llc | Rubber compositions containing viscosity modifier and related methods |
| CN114276857A (en) * | 2021-12-30 | 2022-04-05 | 金丰宏溢科技(佛山)有限公司 | OCP viscosity index improver and preparation method thereof |
Citations (2)
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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 |
-
2011
- 2011-05-13 CN CN201110124569.5A patent/CN102776054B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031195A (en) * | 2013-03-06 | 2014-09-10 | 中国石油天然气股份有限公司 | Preparation method for viscosity index improver |
| US10479881B2 (en) | 2015-06-11 | 2019-11-19 | Bridgestone Americas Tire Operations, Llc | Rubber compositions containing viscosity modifier and related methods |
| US10865291B2 (en) | 2015-06-11 | 2020-12-15 | 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 |
| CN114276857A (en) * | 2021-12-30 | 2022-04-05 | 金丰宏溢科技(佛山)有限公司 | OCP viscosity index improver 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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| CN102776054B (en) | 2014-10-15 |
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