CN104277165B - A kind of preparation method of low viscosity hydrogenated polyvinyl - Google Patents
A kind of preparation method of low viscosity hydrogenated polyvinyl Download PDFInfo
- Publication number
- CN104277165B CN104277165B CN201310248390.XA CN201310248390A CN104277165B CN 104277165 B CN104277165 B CN 104277165B CN 201310248390 A CN201310248390 A CN 201310248390A CN 104277165 B CN104277165 B CN 104277165B
- Authority
- CN
- China
- Prior art keywords
- low viscosity
- temperature
- viscosity
- ionic
- hydrogenated polyvinyl
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Lubricants (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
A kind of preparation method of low viscosity hydrogenated polyvinyl, including: (a) at pressure 0.1～5.0 MPa, temperature 50～150 DEG C, with the polyreaction of ionic liquid catalyst system catalyzed ethylene.B the product of () filtration step (a), controls pressure 0.1～1.0 MPa, temperature 20～75 DEG C, carries out hydrogenation under load catalyst system, obtain low viscosity (V after distillation100℃=1.7～9.7 mm2·s‑1), excellent viscosity temperature characteristic (VI>130), low temperature flow (pour point<60 DEG C), low Noack volatility (<8.5%) and there is the low viscosity hydrogenated polyvinyl artificial oil of the preferable compatibility with lube oil additive.The preparation method advanced person of this kind of low viscosity hydrogenated polyvinyl is simple and direct, low cost, pollution-free, be the low viscosity synthetic lubricant fluid technique of a kind of green.
Description
Technical field
The present invention relates to the preparation method of a kind of low viscosity hydrogenated polyvinyl, belong to polyolefin lubricating oil in syntholube
Field.Described invention includes the preparation of ionic-liquid catalyst, the preparation of low viscosity hydrogenated polyvinyl and post-processing approach thereof.Should
Low viscosity hydrogenated polyvinyl prepared by method has a wide range of applications in fields such as Aeronautics and Astronautics, weapons, precision instrument, machineries
Prospect.
Background technology
Low-viscosity oil is at field tools such as low temperature hydraulic oil, I. C. engine oil, hydraulic transmission oil, auto industry engine oils
It is widely used.At present, the domestic this kind of oil overwhelming majority is still conventional mineral oil, the research and development of synthetic lubricant fluid, factory
Family is few, and technology is the most backward, and product relies primarily on import.Therefore, the preparation method of developmental research low viscosity synthetic lubricant fluid shows
Obtain particularly important.
At present, there is a small amount of preparation method studying low-viscosity oil, mainly poly alpha olefin synthetic lubricant fluid, US 7,
544,850 B2 disclose a kind of method preparing low viscosity poly alpha olefin for raw material with tetradecene, and product has viscosity
The characteristics such as index is high, pour point is low, volatility is little.Shortcoming is that catalyst post processing is complicated, and production cost is high.US 8,207,390
B2 and US 2007/0043248 A1 discloses under transition metal-catalyzed system, and catalysis at least contains the C of 50%4～C24α-alkene
The polymerization of hydrocarbon, the M of productw/MnAbout 1.0～1.4, V100℃< 20 mm2·s-1.US 2009/0326296 A1 discloses by BF3
And BF3The polymerization of catalyst system and catalyzing catalytic mixing alpha-olefin of oligomer composition prepare low viscosity poly alpha olefin lubricating oil, product
Viscosity and Noack volatility low, defect is BF3Equipment corrosion can be caused.CN 102076719 A discloses another kind of low viscous
The preparation method of degree poly alpha olefin, product has low pour point and excellent Noack volatility, but its flash-point is relatively low, limits poly-
The range of application of alpha-olefin.CN 101824354 A have employed BF3-n-butyl alcohol catalyst system and catalyzing passes through catalytic dehydrogenation-alkane separation
Method (Pacol-Olex) produces low viscosity (V100℃=3～5 mm2·s-1) polyolefin synthetic lubricating oil, but the post processing of product
Complexity, and environmental pollution is serious.
As can be seen here, the key technology of synthesis low viscosity synthetic lubricant fluid is raw material and catalyst.Low viscosity is gathered
For alpha olefine synthetic oil, on the one hand, C4～C12Alkene all can be as raw material, and wherein optimum raw material is decene (C10), but C10Purity
The highest and yield is little, often affect quality and the yield of artificial oil；On the other hand, the most homogeneous Lewis of traditional catalyst system
Acid type, Ziegler-Natta, metallocene etc., while bringing great economic benefit, also create post processing complexity, affect hydrogen
Change the problems such as the consumption of catalyst for refining, environmental pollution, etching apparatus.
Ionic liquid suitably can be adjusted according to the feature of reaction and catalytic process itself as novel synthetic lubricant fluid catalyst
The whole zwitterion with modified ion liquid, improves reaction selectivity, reaction rate and yield.Meanwhile, ionic liquid also can be made
Auxiliary agent or " green " succedaneum of organic solvent for catalyst are for catalytic reaction process.As far back as 1993, EP
0558187 A1 discloses employing acidic ion liquid [EMIM] Cl/AlCl3[c(AlCl3=0.67)] catalyzing butene polymerization is anti-
The research answered, product has preferable greasy property, and can be divided into biphase with ionic liquid, it is achieved that catalyst simple
Efficiently separate.WOP 9521872 reports by [EMIM] Cl/AlCl3Ionic-liquid catalyst adds a small amount of helping
Catalyst tetraethyl ammonium salt [NEt4] Cl improve lube oil yield method.Eventually through the structure adjusting ionic-liquid catalyst
Reach to realize the control and regulation of poly alpha olefin lubricating oil viscosity.
Summary of the invention
The present invention has carried out technical optimization on the basis of existing patent 201110366937.7, discloses a kind of low viscosity
The preparation method of hydrogenated polyvinyl, raw materials used ethylene source is extensive, purity is high, and ionic liquid catalyst systems activity is high, technique
The simple and direct advanced person of flow process, cost is relatively low, product water white transparency, environmental protection, and viscosity is low, and viscosity index (VI) is high, pour point and Noack volatilization
Spend low, be suitable as the complete synthesis lubricating oil of low viscosity or lube oil additive product uses.
The technical scheme is that the present invention, under the catalyst system and catalyzing that ionic liquid and promoter are constituted, is catalyzed second
Alkene is polymerized；Under load catalyst system, the hydrofinishing of catalyzed polyethylene compound.
A kind of method preparing low viscosity hydrogenated polyvinyl, specifically comprises the following steps that
(1) preparation of ionic-liquid catalyst: in vacuum glove box, by component A and component B direct reaction or having
Hybrid reaction under machine solvent, and the severe degree reacted by mixing control, wherein, component A with the amount ratio of the material of component B is
2:1～1:4, control reaction temperature 25～55 DEG C, the response time is 2～12 hours, i.e. prepares ionic-liquid catalyst.
Wherein component A is 1,2-dialkylimidazolium, 1,3-dialkylimidazolium；
FormulaIn: R1, R2It is respectively CnH2n+1, n=1～10；
FormulaIn: R1, R2It is respectively CnH2n+1, n=1～10；
Component B is metal halide, and metal halide is AlCl3、ZnCl2、TiCl3、TiCl4、CuCl2、MgCl2。
(2) synthesis of polyethylene: first, by autoclave drying, evacuation, logical nitrogen treatment, it is ensured that reactor
Interior for inert gas shielding environment.Secondly, in autoclave, ionic-liquid catalyst, organic solvent and co-catalysis are added
Agent, and with 100～400 r min-1Rotating speed start stirring.Again, open ethylene valve, be passed through ethylene gas wherein, control
Pressure is 0.1～5.0 MPa, temperature is at 50～150 DEG C, polyreaction 20～70 hours, i.e. obtains low viscosity polyethylene thick
Product, then temperature of reaction kettle is down to room temperature, product is staticly settled, filters to isolate ionic-liquid catalyst and remnants thereof,
Obtain low viscosity polyethylene.
In above-mentioned steps, promoter is MAO, compound alkyl aluminum, RnAlX3-n, dense H2SO4, HCl gas；
RnAlX3-nIn X be F, Cl, Br, I, n=1,2,3 etc..
In above-mentioned steps, meet m(ionic-liquid catalyst): m(organic solvent): m(promoter)=10: 100
: 1～30: 600: 1.
(3) hydrogenation of low viscosity polyethylene: first, hydrogenation reaction cauldron drying, evacuation, logical nitrogen treatment, it is ensured that anti-
It is inert gas shielding environment in answering still.Secondly, in the presence of load type catalyst system, in autoclave, add step
(2) product and organic solvent, and with more than 300 r min-1Rotating speed start stirring.Again, open hydrogen valve, wherein
Being passed through hydrogen, control pressure is 0.1～1.0 MPa, temperature is at 20～75 DEG C, and hydrogenation reaction 2～48 hours, finally by steaming
Evaporate, obtain low viscosity hydrogenated polyvinyl synthetic lubricant fluid product.
In above-mentioned steps, hydrogenation used catalyst is that nickel-loaded series catalysts, Supported Pt Nanoparticles series catalysts or supported palladium system urge
Agent, and meet m(supported catalyst): m(organic solvent)=1: 15～1: 100.During this reaction, insatiable hunger
Typically it is lowered more than 95% with the amount of degree.
In step (1), step (2) and step (3), organic solvent is the nonpolar or polarity after processed relatively
Little solvent, organic solvent is chlorobenzene, toluene, dichloromethane, chloroform, hexamethylene or carbon tetrachloride etc..
The present invention compared with prior art has the advantage that ionic-liquid catalyst catalysis activity is strong, service life is long,
Non-volatility, little to the corrosivity of equipment, easily and sub polyethylene from.The preparation method of this kind of low viscosity hydrogenated polyvinyl, has
Preparation process is simple and direct, efficient, and required production equipment and reagent price are relatively inexpensive, and production cost is relatively low.Meanwhile, prepared by this method
Low viscosity hydrogenated polyvinyl except having the excellent features such as colorless and odorless, safety non-toxic, environmental protection, also there is viscosity low,
Viscosity index (VI) is high, and the characteristics such as pour point is low, Noack volatility is low, are the preparation methoies of a kind of efficient low viscosity hydrogenated polyvinyl.
Detailed description of the invention
Below by specific embodiment, technical scheme is described in further detail, but the application of the present invention
It is not only limited to the scope of embodiment.
Embodiment 1
(1) preparation of ionic-liquid catalyst: in vacuum glove box, by 1,2-methylimidazole and AlCl3At hexamethylene
Hybrid reaction under alkane, and the severe degree reacted by mixing control, wherein, meet n(1,2-methylimidazole): n
(AlCl3)=1: 3, controlling reaction temperature is 45 DEG C, and the response time is 10 hours, i.e. prepares ionic-liquid catalyst.
(2) synthesis of polyethylene: first, by 2.0 L autoclave dryings, evacuation, logical nitrogen treatment, it is ensured that anti-
It is inert gas shielding environment in answering still.Secondly, by m(ionic-liquid catalyst): m(hexamethylene): m(MAO)=15:
The ratio of 250: 1, is added in autoclave, and with 300 r min-1Rotating speed stirring.Again, open ethylene valve,
Be passed through ethylene gas wherein, control pressure be 0.5 MPa, temperature be at 120 DEG C, polyreaction 18 hours, i.e. obtain primiparity
Thing polyethylene.Again temperature of reaction kettle is down to room temperature, product is staticly settled, filters to isolate ionic-liquid catalyst and residual
Remaining, i.e. obtain low viscosity polyethylene.
(3) hydrogenation of low viscosity polyethylene: first, at 10.0 L hydrogenation reaction cauldron dryings, evacuation, logical nitrogen
Reason, it is ensured that be inert gas environment in reactor.Secondly, by m(loaded palladium catalyst): m(hexamethylene)=the ratio of 1: 20
Example, is added in reactor, and with 350 r min-1Rotating speed stirring.Again, open hydrogen valve, be passed through hydrogen wherein,
Control pressure be 0.5 MPa, temperature be at 45 DEG C, hydrogenation reaction 10 hours, then product is distilled, obtains low viscosity hydrogenation
Polyethylene synthetic lubricant fluid/lube oil additive product, yield is 77.2%.This low viscosity hydrogenated polyvinyl is the motion of 40 DEG C
Viscosity is 5.8 mm2·s-1, it is 1.7 mm at the kinematic viscositys of 100 DEG C2·s-1, pour point is-73 DEG C, and Noack volatility is
8.3%。
Embodiment 2
(1) preparation of ionic-liquid catalyst: in vacuum glove box, by 1-methyl-2-second Methylimidazole. and ZnCl2?
Hybrid reaction under hexamethylene, and the severe degree reacted by mixing control, wherein, meet n(1-methyl-2-second methyl miaow
Azoles): n(ZnCl2)=2: 5, reaction temperature controls at 40 DEG C, and the response time is 10 hours, i.e. prepares ionic liquid-catalyzed
Agent.
(2) synthesis of polyethylene: first, by 2.0 L autoclave dryings, evacuation, logical nitrogen treatment, it is ensured that anti-
It is inert gas shielding environment in answering still.Secondly, by m(ionic-liquid catalyst), m(dichloromethane), m(AlEt2Cl-AlEt3)
The ratio of=12: 300: 1, is added in autoclave, and with 250 r min-1Rotating speed stirring.Again, open
Ethylene valve, is passed through ethylene gas wherein, control pressure be 0.7 MPa, temperature be at 100 DEG C, polyreaction 20 hours, i.e. obtain
Obtain head product polyethylene.Again temperature of reaction kettle is down to room temperature, product is staticly settled, filters to isolate ionic-liquid catalyst
And remaining, obtain low viscosity polyethylene.
(3) hydrogenation of low viscosity polyethylene: first, at 10.0 L autoclave dryings, evacuation, logical nitrogen
Reason, it is ensured that for inert gas shielding environment in reactor.Secondly, by m(loaded palladium catalyst): m(dichloromethane)=3: 10
Ratio, be added in autoclave, and with 400 r min-1Rotating speed stirring.Open hydrogen valve again, be passed through wherein
Hydrogen, control pressure 0.5 MPa, temperature be at 30 DEG C, hydrogenation reaction 12 hours, then product is distilled, obtains low viscosity
Hydrogenated polyvinyl synthetic lubricant fluid/lube oil additive product, yield is 87.3%.This low viscosity hydrogenated polyvinyl is 40 DEG C of fortune
Kinetic viscosity is 6.7 mm2·s-1, the kinematic viscosity of 100 DEG C is 2.2mm2·s-1, pour point is-68 DEG C, and Noack volatility is
8.0%。
Embodiment 3
(1) preparation of ionic-liquid catalyst: in vacuum glove box, by 1-ethyl-2-ethyl imidazol(e) and TiCl4At ring
Hybrid reaction under hexane, and the severe degree reacted by mixing control, wherein, meet n(1-ethyl-2-ethyl imidazol(e)): n
(TiCl4)=2: 7, reaction temperature controls at 45 DEG C, and the response time is 10 hours, i.e. prepares ionic-liquid catalyst.
(2) synthesis of polyethylene: first, by 10.0 L autoclave dryings, evacuation, logical nitrogen treatment, it is ensured that
For inert gas shielding environment in reactor.Secondly, by m(ionic-liquid catalyst): m(chloroform): m(Et2AlCl) =10
: the ratio of 200: 1, it is added in autoclave, and with 200 r min-1Rotating speed stirring.Again, ethylene is opened
Valve, is passed through ethylene gas wherein, control pressure be 0.8 MPa, temperature be at 85 DEG C, polyreaction 20 hours, at the beginning of i.e. obtaining
Product polyethylene.Again temperature of reaction kettle is down to room temperature, product is staticly settled, filter to isolate ionic-liquid catalyst and
Remnants, i.e. obtain low viscosity polyethylene.
(3) hydrogenation of low viscosity polyethylene: first, at 10.0 L autoclave dryings, evacuation, logical nitrogen
Reason, it is ensured that for inert gas shielding environment in reactor.Secondly, by m(supported nickel catalyst): m(chloroform)=the ratio of 1: 9
Example, is added in autoclave, and is 400 r min with rotating speed-1Stirring.Again, open hydrogen valve, be passed through wherein
Hydrogen, control pressure be 1.0 MPa, temperature be at 65 DEG C, hydrogenation reaction 3 hours, then product is distilled, obtains low viscosity
Hydrogenated polyvinyl synthetic lubricant fluid/lube oil additive product, yield is 89.1%.This low viscosity hydrogenated polyvinyl is at 40 DEG C
Kinematic viscosity is 9.3 mm2·s-1, the kinematic viscosity of 100 DEG C is 2.7 mm2·s-1, viscosity index (VI) VI=130, pour point-65
DEG C, Noack volatility is 6.8%.
Embodiment 4
(1) preparation of ionic-liquid catalyst: in vacuum glove box, by 1-methyl-3-Methylimidazole. and AlCl3At ring
Hybrid reaction under hexane, and the severe degree reacted by mixing control, wherein, meet n(1-methyl-3-Methylimidazole .): n
(AlCl3)=1: 3, reaction temperature controls at 45 DEG C, and the response time is 10 hours, i.e. prepares ionic-liquid catalyst.
(2) synthesis of polyethylene: first, by 10.0 L autoclave dryings, evacuation, logical nitrogen treatment, it is ensured that
For inert gas shielding environment in reactor.Secondly, by m(ionic-liquid catalyst): m(carbon tetrachloride): m(MAO)=15
: the ratio of 200:1, it is added in autoclave, and with 180 r min-1Rotating speed stirring.Again, ethylene is opened
Valve, is passed through ethylene gas wherein, control pressure be 1.0 MPa, temperature be at 65 DEG C, polyreaction 24 hours, at the beginning of i.e. obtaining
Product polyethylene.Again temperature of reaction kettle is down to room temperature, product is staticly settled, filter to isolate ionic-liquid catalyst and
Remnants, obtain low viscosity polyethylene.
(3) hydrogenation of low viscosity polyethylene: first, at 10.0 L autoclave dryings, evacuation, logical nitrogen
Reason, it is ensured that for inert gas shielding environment in reactor.Secondly, by m(supported nickel catalyst): m(carbon tetrachloride)=1: 10
Ratio, be added in autoclave, and with 450 r min-1Rotating speed stirring.Again, open hydrogen valve, wherein
Be passed through hydrogen, control pressure be 1.0 MPa, temperature be at 40 DEG C, hydrogenation reaction 8 hours, then product is distilled, obtains low
Viscosity hydrogenated polyvinyl synthetic lubricant fluid/lube oil additive product, yield is 90.5%.This low viscosity hydrogenated polyvinyl is 40
DEG C kinematic viscosity be 11.3 mm2·s-1, the kinematic viscosity of 100 DEG C is 3.1 mm2·s-1, viscosity index (VI) VI=138, incline
Point-63 DEG C, Noack volatility is 5.6%.
Embodiment 5
(1) preparation of ionic-liquid catalyst: in vacuum glove box, by 1-methyl-3-ethyl imidazol(e) and AlCl3At ring
Hybrid reaction under hexane, and the severe degree reacted by mixing control, wherein, meet n(1-methyl-3-ethyl imidazol(e)): n
(AlCl3)=1: 3, reaction temperature controls at 40 DEG C, and the response time is 10 hours, i.e. prepares ionic-liquid catalyst.
(2) synthesis of polyethylene: first, by 10.0 L autoclave dryings, evacuation, logical nitrogen treatment, it is ensured that
For inert gas shielding environment in reactor.Secondly, by m(ionic-liquid catalyst): m(hexamethylene): the dense H of m(2SO4)=10
: the ratio of 200: 1, it is added in autoclave, and with 150 r min-1Rotating speed stirring.Again, ethylene is opened
Valve, is passed through ethylene gas wherein, control pressure be 1.2 MPa, temperature be at 60 DEG C, polyreaction 30 hours, i.e. obtain thick
Product polyethylene.Again temperature of reaction kettle is down to room temperature, product is staticly settled, filter to isolate ionic-liquid catalyst and
Remnants, i.e. obtain low viscosity polyethylene.
(3) hydrogenation of low viscosity polyethylene: first, at 10.0 L autoclave dryings, evacuation, logical nitrogen
Reason, it is ensured that for inert gas shielding environment in reactor.Secondly, by m(load platinum catalyst): m(hexamethylene)=1: 10
Ratio, is added in autoclave, and with 500 r min-1Rotating speed stirring.Again, open hydrogen valve, lead to wherein
Enter hydrogen, control pressure be 0.9 MPa, temperature be at 45 DEG C, hydrogenation reaction 12 hours, then product is distilled, obtains low
Viscosity hydrogenated polyvinyl synthetic lubricant fluid/lube oil additive product, yield is 92.1%.This low viscosity hydrogenated polyvinyl is 40
DEG C kinematic viscosity be 33.0 mm2·s-1, the kinematic viscosity of 100 DEG C is 6.2 mm2·s-1, viscosity index (VI) VI=145, incline
Point-65 DEG C, Noack volatility is 4.5%.
Embodiment 6
(1) preparation of ionic-liquid catalyst: in vacuum glove box, by 1-ethyl-3-ethyl imidazol(e) and ZnCl2At ring
Hybrid reaction under hexane, and the severe degree reacted by mixing control, wherein, meet n(1-ethyl-3-ethyl imidazol(e)): n
(ZnCl2)=1: 2, reaction temperature controls at 40 DEG C, and the response time is 8 hours, i.e. prepares ionic-liquid catalyst.
(2) synthesis of polyethylene: first, by 10.0 L autoclave dryings, evacuation, logical nitrogen treatment, it is ensured that
For inert gas shielding environment in reactor.Secondly, by m(ionic-liquid catalyst): m(dichloromethane): m(AlEt2Cl-
AlEt3The ratio of)=12: 200: 1, is added in autoclave, and with 160 r min-1Rotating speed stirring.Again
Secondary, open ethylene valve, be passed through ethylene gas wherein, control pressure be 2.5 MPa, temperature be at 50 DEG C, polyreaction 32 little
Time, i.e. obtain crude product polyethylene.Again temperature of reaction kettle is down to room temperature, product is staticly settled, filters to isolate ionic liquid
Body catalyst and remnants thereof, i.e. obtain low viscous polyethylene.
(3) hydrogenation of low viscosity polyethylene: first, at 10.0 L autoclave dryings, evacuation, logical nitrogen
Reason, it is ensured that for inert gas shielding environment in reactor.Secondly, by m(loaded palladium catalyst): m(dichloromethane)=13:
The ratio of 90, is added in autoclave, and with 450 r min-1Rotating speed stirring.Again, hydrogen valve, Xiang Qi are opened
In be passed through hydrogen, control pressure be 1.0 MPa, temperature be at 40 DEG C, hydrogenation reaction 8 hours, then product is distilled, to obtain final product
Low viscosity hydrogenated polyvinyl synthetic lubricant fluid/lube oil additive product, yield is 93.0%.This low viscosity hydrogenated polyvinyl exists
The kinematic viscosity of 40 DEG C is 40.0 mm2·s-1, the kinematic viscosity of 100 DEG C is 7.0 mm2·s-1, viscosity index (VI) is VI=148,
Pour point is-62 DEG C, and Noack volatility is 4.0%.
Experimental result is shown in Table 1
The performance of table 1 low viscosity hydrogenated polyvinyl
The above, be only presently preferred embodiments of the present invention, not impose any restrictions the present invention, every according to the present invention
Any simple modification, change and the equivalent structure change that above example is made by technical spirit, all still falls within skill of the present invention
In the protection domain of art scheme.
Claims (6)
1. the preparation method of a low viscosity hydrogenated polyvinyl, it is characterised in that the method concrete operations are as follows: (1) ionic liquid
The preparation of body catalyst: in vacuum glove box, by component A and component B direct reaction or under organic solvent hybrid reaction, and
React severe degree by mixing control, wherein, meet the amount of component A and the material of component B ratio for 2:1～1:4, control reaction
Temperature 25～55 DEG C, the response time is 2～12 hours, i.e. prepares ionic-liquid catalyst；(2) synthesis of polyethylene: be full of
The autoclave of nitrogen adds ionic-liquid catalyst, organic solvent and promoter, is passed through ethylene gas, and with 100
～400 r min-1Rotating speed start stirring, control pressure be 0.1～5.0 MPa, temperature be 50～150 DEG C and polyreaction
Time is 20～70 hours, i.e. obtains low viscosity polyethylene head product；(3) hydrogenation of low viscosity polyethylene: at load hydrogenation
In the presence of catalyst system, the low viscosity that addition organic solvent and step (2) prepare in the hydrogenation reaction cauldron of full nitrogen is gathered
Ethylene head product, is passed through hydrogen, with more than 300 r min-1Rotating speed stirring, control pressure be 0.1～1.0 MPa, temperature be
20～75 DEG C, the hydrogenation time be 2～48 hours, low viscosity hydrogenated polyvinyl can be obtained, finally by distillation, obtain
Low viscosity hydrogenated polyvinyl synthetic lubricant fluid product；
Component A is 1,2-dialkylimidazolium or 1,3-dialkylimidazolium, and described component B is metal halide, metal halide
For AlCl3、ZnCl2、TiCl3、TiCl4、CuCl2Or MgCl2；
In described step (2), m(ionic-liquid catalyst): m(organic solvent): m(promoter)=10: 100: 1～
30: 600: 1, in described step (3), m(loaded catalyst): m(organic solvent)=1: 15～1: 100.
The most in accordance with the method for claim 1, it is characterised in that: in step (1), step (2), step (3), organic solvent is equal
For the solvent less through the nonpolar of processed or polarity, organic solvent be benzene, toluene, dichloromethane, chloroform, hexamethylene or
Carbon tetrachloride.
The most in accordance with the method for claim 1, it is characterised in that: in step (2), promoter is MAO, compound alkane
Base aluminum, RnAlX3-n, dense H2SO4Or HCl gas；RnAlX3-nIn X be F, Cl, Br, I, n=1,2,3.
The most in accordance with the method for claim 1, the low viscosity hydrogenated polyvinyl prepared has 1.7 to 9.7 at 100 DEG C
mm2·s-1Kinematic viscosity；Described kinematic viscosity is measured by GB/T 265-1988 (2004).
The most in accordance with the method for claim 1, the low viscosity hydrogenated polyvinyl prepared has viscosity index (VI) and is more than 130
Viscosity-temperature characteristics；Described viscosity index (VI) is measured by GB/T 1995-1998 (2004).
The most in accordance with the method for claim 1, the low viscosity hydrogenated polyvinyl prepared has the pour point of-60 to-78 DEG C；
Described pour point is measured by GB/T 3535-2006.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310248390.XA CN104277165B (en) | 2013-06-21 | 2013-06-21 | A kind of preparation method of low viscosity hydrogenated polyvinyl |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310248390.XA CN104277165B (en) | 2013-06-21 | 2013-06-21 | A kind of preparation method of low viscosity hydrogenated polyvinyl |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104277165A CN104277165A (en) | 2015-01-14 |
| CN104277165B true CN104277165B (en) | 2016-10-12 |
Family
ID=52252550
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310248390.XA Active CN104277165B (en) | 2013-06-21 | 2013-06-21 | A kind of preparation method of low viscosity hydrogenated polyvinyl |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104277165B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104449901A (en) * | 2013-09-18 | 2015-03-25 | 西安艾姆高分子材料有限公司 | Environmentally friendly biodiesel/petrochemical diesel heat value increasing agent |
| CN112725054B (en) * | 2019-10-28 | 2023-10-20 | 南京中科康润新材料科技有限公司 | Process method for directly synthesizing high-performance high-viscosity base oil by polymerization of low-carbon olefin |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6156854A (en) * | 1997-02-06 | 2000-12-05 | Fina Technology, Inc. | Method of olefin polymerization utilizing hydrogen pulsing, products made therefrom, and method of hydrogenation |
| CN1882613A (en) * | 2003-11-14 | 2006-12-20 | 托塔尔石油化学产品研究弗吕公司 | Heterogenisation of polymerisation catalysts by ionic liquids |
| CN101434666A (en) * | 2008-12-17 | 2009-05-20 | 中国科学院长春应用化学研究所 | Magnesium chloride/mesoporous molecular sieve bisupported Ziegler-Natta polyethylene catalyst, preparation and use |
| CN102786435A (en) * | 2011-05-16 | 2012-11-21 | 中国科学院上海有机化学研究所 | Catalysis systems for preparing highly branched alkane by using olefin |
-
2013
- 2013-06-21 CN CN201310248390.XA patent/CN104277165B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6156854A (en) * | 1997-02-06 | 2000-12-05 | Fina Technology, Inc. | Method of olefin polymerization utilizing hydrogen pulsing, products made therefrom, and method of hydrogenation |
| CN1882613A (en) * | 2003-11-14 | 2006-12-20 | 托塔尔石油化学产品研究弗吕公司 | Heterogenisation of polymerisation catalysts by ionic liquids |
| CN101434666A (en) * | 2008-12-17 | 2009-05-20 | 中国科学院长春应用化学研究所 | Magnesium chloride/mesoporous molecular sieve bisupported Ziegler-Natta polyethylene catalyst, preparation and use |
| CN102786435A (en) * | 2011-05-16 | 2012-11-21 | 中国科学院上海有机化学研究所 | Catalysis systems for preparing highly branched alkane by using olefin |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104277165A (en) | 2015-01-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102666806B (en) | For the production of the method for novel synthetic base oil material | |
| JP2019508227A (en) | Antifouling oligomerization catalyst system | |
| US10927052B2 (en) | Decene oligomers | |
| WO2016058559A1 (en) | New polyolefin catalyst and use thereof | |
| JP2013512328A (en) | Production of oligomers from nonene | |
| CN104277165B (en) | A kind of preparation method of low viscosity hydrogenated polyvinyl | |
| JP6329129B2 (en) | Alpha-olefin polymer and method for producing hydrogenated alpha-olefin polymer | |
| CN104560180B (en) | Lube base oil and/or the continuous producing method of solvent naphtha and device | |
| CN102875707A (en) | Preparation method of catalyst component for ethylene polymerization or copolymerization and catalyst thereof | |
| CN105829268A (en) | Method for making polyolefins using aluminum halide catalyzed oligomerization of olefins | |
| CN110330529B (en) | Pyridine imine palladium complex for preparing synthetic lubricating oil from alpha-olefin, and preparation method and application thereof | |
| CN102070733B (en) | Method for preparing synthetic hydrocarbon | |
| CN105272809B (en) | Removal method of oxygen-containing compounds in coal alpha-olefins | |
| CN101565651A (en) | Method for preparing high viscosity lubricating oil | |
| CN110078753A (en) | A kind of synthetic method of metallocene catalysis agent aid and its application in 1- decene polymerization process | |
| CN109369835A (en) | For the cyclopentadienyl rare-earth metal carbon monoxide-olefin polymeric of alpha-olefine polymerizing and its application | |
| CN114075305B (en) | Polyolefin lubricating oil base oil and preparation method thereof | |
| CN109369836A (en) | A kind of cyclopentadienyl rare-earth metal carbon monoxide-olefin polymeric and its application containing heterocycle structure | |
| CN103525456A (en) | Synthetic hydrocarbon base oil prepared through coal-based alpha olefin | |
| CN110041457B (en) | Alpha-olefin polymerization catalyst, preparation method thereof and alpha-olefin polymerization method | |
| CN103122265A (en) | Novel polyethylene synthetic lubricating oil/lubricating oil additive and preparation method thereof | |
| CN101723780A (en) | Method for preparing synthetic hydrocarbon | |
| WO2021029939A1 (en) | Processes for producing poly alpha olefins and apparatuses therefor | |
| EP4010307A1 (en) | Processes for producing poly alpha olefins and method of analysis and apparatuses therefor | |
| CN113185998B (en) | Narrow-distribution PAO base oil taking C8-C10 alpha-olefin tetramer as main component and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |