CN102079684B - Method for catalyzing complete hydrogenation of polyalphaolefin into saturated alkane - Google Patents
Method for catalyzing complete hydrogenation of polyalphaolefin into saturated alkane Download PDFInfo
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- CN102079684B CN102079684B CN 201010574582 CN201010574582A CN102079684B CN 102079684 B CN102079684 B CN 102079684B CN 201010574582 CN201010574582 CN 201010574582 CN 201010574582 A CN201010574582 A CN 201010574582A CN 102079684 B CN102079684 B CN 102079684B
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Abstract
The invention belongs to the technical field of fine chemistry, in particular to a method for complete hydrogenation of polyalphaolefin into saturated alkane. The method synthesizes a Ni/nano Al2O3 catalyst by using an immersion process. The polyalphaolefin can be catalytically reduced into saturated alkane under the conditions that: the Ni/nano Al2O3 catalyst is used, the reaction temperature is 60 to 200 DEG C, the pressure range is from 1.0 to 6.0Mpa, the liquid hourly space velocity is 0.4 to 0.8<-1>, and the molar ratio of hydrogen to polyalphaolefin is 5 to 20. The method of the invention is simple in process and low in cost and has a bright application prospect.
Description
Technical field
The invention belongs to the fine chemical technology field, be specifically related to a kind of Ni/ nanometer Al of loading type
2O
3Catalyzer is used for the method for the synthetic saturated alkane of the complete hydrogenation of a kind of polyalphaolefin.
Background technology
After the seventies in 20th century, along with the technical progress of various engines and other mechanical means and urgent day by day " energy-conservation " " environmental protection " requirement, salient featuress such as the sticking warm nature of lubricating oil, volatility, thermal oxidation stability have also been proposed harsh day by day requirement, the capability and performance of natural mineral matter base oil is near the limit, is difficult to modulating performance, product with a higher standard again.This has just directly promoted the development of synthetic base oil.Because lubricating oil specification, particularly the I. C. engine oil specification is stricter in recent years, and many indexs only depend on mineral oil to be difficult to satisfy the requirement of new spec, impels people that the interest of synthetic oil is heightened, and has also promoted the demand growth of ucon oil.
The long-chain saturated alkane has been compared many advantages as the engine oil of base oil modulation with the mineral oil engine oil.The thermostability and the oxidation stability that at first are this alkene obviously are better than mineral oil, can prolong the oil draining period, have reduced maintenance cost and have reduced shutdown period.In addition, when using this ucon oil, the additive compatibility commonly used with the mineral substance base oil is good, and can reduce the consumption of additive, or with more cheap additive, this can dwindle the price variance of this ucon oil and mineral oil origin vehicular engine oil.
Ucon oil has also that operating temperature range is wide, viscosity-temperature characteristics can be good, pour point is low, viscosity index is high, vaporization losses is little, low volatility, lightning, point of ignition, spontaneous ignition temperature height, non-hygroscopic under the high temperature, hydrolysis stability is good, and shear stability is good, to the equipment non-corrosiveness.In addition, little to engine wear under low temperature and hot conditions, carbon distribution is few, and is biodegradable, and long service life, the efficient height, and coking is few, nontoxic and skin had characteristics such as immersional wetting.
In the process of producing ucon oil, wish polyalphaolefin is carried out hydrogenation, make olefinic double bonds remaining in the molecule saturated, to guarantee chemical stability and the thermostability of product.The quality of this step for product plays crucial effects.If do not carry out this step hydrogenation reaction, the life-span can be very short in the engine of running rapidly or in the steam turbine of high temperature for alkene.Even if not in such environment, airborne oxygen also can with destroy two keys, thereby the capability and performance of product is reduced greatly, lost its original meaning.
The catalyzer that is used for the polyalphaolefin hydrogenation at present mainly contains the nickel-alumina catalyst of Raney's nickel and employing coprecipitation method.By comparison, adopt pickling process to produce catalyzer and have the saving metallic nickel, the advantage that surface-area is big.Therefore, the invention provides and a kind of active component nickel is dispersed on the nano aluminium oxide method that obtains the big outside surface nickel catalyzator of high dispersive, and be applied to the polyalphaolefin hydrogenation.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of technology, the method for the complete hydrogenation synthesizing alkanes of catalysis polyalphaolefin with low cost.
The method of the complete hydrogenation synthesizing alkanes of catalysis polyalphaolefin provided by the invention is at the Ni/ of loading type nanometer Al
2O
3Under the effect of catalyzer, polyalphaolefin is reduced into the process of alkane fully.Catalyzed reaction is being carried out in the gas-liquid fixed catalytic reaction bed continuously.Its reaction formula is:
C
nH
2n + H
2 → C
nH
2n+2 (n=20—100)
The present invention is at the Ni/ of loading type nanometer Al
2O
3Under the catalyst action, polyalphaolefin with enter catalytic bed after hydrogen mixes by a certain percentage, hydrogenating reduction becomes alkane fully, its actual conditions is:
(1) temperature range of this catalyzed reaction is 60-200
oC;
(2) pressure range of catalyzed reaction is 1.0-6.0 MPa;
(3) the liquid hourly space velocity scope is 0.4-0.8 h
-1
(4) hydrogen and polyalphaolefin mol ratio are 5-20.
Among the present invention, the Ni/ nanometer Al of described loading type
2O
3Catalyzer is by pickling process load nickelous nitrate, then by high temperature air roasting generation NiO/ nanometer Al at the alumina material with nano-scale particle
2O
3Catalyzer obtains Ni/ nanometer Al with hydrogen reducing before using
2O
3Catalyzer.Its concrete preparation method is as follows:
Ni/ nanometer Al according to loading type
2O
3The content value of nickel takes by weighing nickelous nitrate in the catalyzer, uses dissolved in distilled water.Add nano aluminium oxide then, mix the back fully in ultrasonic machine ultrasonic 5-60 minute.At room temperature ventilation ageing 5-24h.60-70 ℃ of following air seasoning, obtain dry mixture then, add thermal bake-out again in retort furnace, Heating temperature is 400-600 ℃, and roasting time is 1-10h.Before the use, with catalyzer at hydrogen nitrogen mixed gas (wherein, H
2Volume content 1%-100%) exists down in 200
OC-500
oThe C scope is reduced, and obtains Ni/Al
2O
3Catalyzer.
The Ni/ nanometer Al of described loading type
2O
3Catalyzer, its carrier are the nanometer gama-alumina, and metallic nickel is catalytic active component.Wherein the charge capacity of metallic nickel is 1wt%-10wt%.
Big, active high, the good stability of the catalyst surface area that the present invention uses.
Described polyalphaolefin, molecular formula are C
nH
2n, wherein n is carbonatoms, is 20-100.
The present invention uses simple method, has realized that the complete hydrogenating reduction of polyalphaolefin becomes alkane, makes the olefinic double bonds in the molecule saturated, and to guarantee chemical stability and the thermostability of product, the transformation efficiency of polyalphaolefin can reach 100%.The catalyst preparation process that the present invention uses is simple, with low cost.Therefore, the present invention has a good application prospect.
Embodiment
Further describe the present invention below by example.
Embodiment 1
Ni(1%)/nanometer Al
2O
3Catalyzer prepares as follows:
Take by weighing with the weight ratio is nickelous nitrate: water: nano aluminium oxide=0.5:13.3:10, use dissolved in distilled water.Add nano aluminium oxide then, mix the back fully in ultrasonic machine ultrasonic 5-60 minute.After mixing fully, at room temperature ventilation ageing 5-24h.70 ℃ of following air seasonings, obtain adding thermal bake-out after the dry mixture in retort furnace then, Heating temperature is 400-600 ℃.Roasting time is 1-10h.Before the use, with catalyzer at hydrogen nitrogen mixed gas (H
2Content 1%-100%) exists down in 200
OC-500
oThe C scope is reduced, and obtains Ni/Al
2O
3Catalyzer.
Restrain the Ni(1% that gets ready with 10)/nanometer Al
2O
3The catalyzer diameter of packing into is in 8 millimeters the stainless steel reaction pipe, with polyalphaolefin (C
100H
200) feed in the reaction tubes after mixing with hydrogen, entering the catalytic bed reaction, temperature of reaction is 200 ℃, and reaction system pressure is 1.0Mpa, and liquid hourly space velocity is 0.8, and hydrogen and polyalphaolefin mol ratio are 5, polyalphaolefin (C
100H
200) transformation efficiency is 100%.
Embodiment 2
Ni(3%)/nanometer Al
2O
3Catalyzer prepares as follows:
Take by weighing with the weight ratio is nickelous nitrate: water: nano aluminium oxide=1.5:13:10, use dissolved in distilled water.Add nano aluminium oxide then, mix the back fully in ultrasonic machine ultrasonic 5-60 minute.After mixing fully, at room temperature ventilation ageing 5-24h.70 ℃ of following air seasonings, obtain adding thermal bake-out after the dry mixture in retort furnace then, Heating temperature is 400-600 ℃.Roasting time is 1-10h.Before the use, with catalyzer at hydrogen nitrogen mixed gas (H
2Content 1%-100%) exists down in 200
OC-500
oThe C scope is reduced, and obtains Ni/Al
2O
3Catalyzer.
Restrain the Ni(3% that gets ready with 10)/nanometer Al
2O
3The catalyzer diameter of packing into is in 8 millimeters the stainless steel reaction pipe, with polyalphaolefin (C
80H
160) feed in the reaction tubes after mixing with hydrogen, entering the catalytic bed reaction, temperature of reaction is 160 ℃, and reaction system pressure is 5.0Mpa, and liquid hourly space velocity is 0.8, and hydrogen and polyalphaolefin mol ratio are 15, polyalphaolefin (C
80H
160) transformation efficiency is 100%.
Embodiment 3
Ni(5%)/nanometer Al
2O
3Catalyzer prepares as follows:
Take by weighing with the weight ratio is nickelous nitrate: water: nano aluminium oxide=2.5:12.6:10, use dissolved in distilled water.Add nano aluminium oxide then, mix the back fully in ultrasonic machine ultrasonic 5-60 minute.After mixing fully, at room temperature ventilation ageing 5-24h.70 ℃ of following air seasonings, obtain adding thermal bake-out after the dry mixture in retort furnace then, Heating temperature is 400-600 ℃.Roasting time is 1-10h.Before the use, with catalyzer at hydrogen nitrogen mixed gas (H
2Content 1%-100%) exists down in 200
OC-500
oThe C scope is reduced, and obtains Ni/Al
2O
3Catalyzer.
Restrain the Ni(5% that gets ready with 10)/nanometer Al
2O
3The catalyzer diameter of packing into is in 8 millimeters the stainless steel reaction pipe, with polyalphaolefin (C
60H
120) feed in the reaction tubes after mixing with hydrogen, entering the catalytic bed reaction, temperature of reaction is 140 ℃, and reaction system pressure is 4.0Mpa, and liquid hourly space velocity is 0.7, and hydrogen and polyalphaolefin mol ratio are 13, polyalphaolefin (C
60H
120) transformation efficiency is 100%.
Embodiment 4
Ni(7%)/nanometer Al
2O
3Catalyzer prepares as follows:
Take by weighing with the weight ratio is nickelous nitrate: water: nano aluminium oxide=3.5:12.4:10, use dissolved in distilled water.Add nano aluminium oxide then, mix the back fully in ultrasonic machine ultrasonic 5-60 minute.After mixing fully, at room temperature ventilation ageing 5-24h.70 ℃ of following air seasonings, obtain adding thermal bake-out after the dry mixture in retort furnace then, Heating temperature is 400-600 ℃.Roasting time is 1-10h.Before the use, with catalyzer at hydrogen nitrogen mixed gas (H
2Content 1%-100%) exists down in 200
OC-500
oThe C scope is reduced, and obtains Ni/Al
2O
3Catalyzer.
Restrain the Ni(7% that gets ready with 10)/nanometer Al
2O
3The catalyzer diameter of packing into is in 8 millimeters the stainless steel reaction pipe, with polyalphaolefin (C
40H
80) feed in the reaction tubes after mixing with hydrogen, entering the catalytic bed reaction, temperature of reaction is 100 ℃, and reaction system pressure is 3.0Mpa, and liquid hourly space velocity is 0.6, and hydrogen and polyalphaolefin mol ratio are 10, polyalphaolefin (C
40H
80) transformation efficiency is 100%.
Embodiment 5
Ni(10%)/nanometer Al
2O
3Catalyzer prepares as follows:
Take by weighing with the weight ratio is nickelous nitrate: water: nano aluminium oxide=5:11.6:10, use dissolved in distilled water.Add nano aluminium oxide then, mix the back fully in ultrasonic machine ultrasonic 5-60 minute.After mixing fully, at room temperature ventilation ageing 5-24h.70 ℃ of following air seasonings, obtain adding thermal bake-out after the dry mixture in retort furnace then, Heating temperature is 400-600 ℃.Roasting time is 1-10h.Before the use, with catalyzer at hydrogen nitrogen mixed gas (H
2Content 1%-100%) exists down in 200
OC-500
oThe C scope is reduced, and obtains Ni/Al
2O
3Catalyzer.
Restrain the Ni(10% that gets ready with 10)/nanometer Al
2O
3The catalyzer diameter of packing into is in 8 millimeters the stainless steel reaction pipe, with polyalphaolefin (C
20H
40) feed in the reaction tubes after mixing with hydrogen, entering the catalytic bed reaction, temperature of reaction is 60 ℃, and reaction system pressure is 6.0Mpa, and liquid hourly space velocity is 0.4, and hydrogen and polyalphaolefin mol ratio are 20, polyalphaolefin (C
20H
40) transformation efficiency is 100%.
Claims (2)
1. the method for the synthetic saturated alkane of the complete hydrogenation of catalysis polyalphaolefin is characterized in that at the Ni/ of loading type nanometer Al
2O
3Under the existence of catalyzer, polyalphaolefin is hydrogenated to alkane fully, and the fixed bed that polyalphaolefin and hydrogen together enter loading catalyst during reaction reacts, and reaction conditions is:
(1) temperature range of this catalyzed reaction is 60
oC-200
oC;
(2) pressure range of catalyzed reaction is 1.0 MPa-6.0 MPa;
(3) the liquid hourly space velocity scope is 0.4-0.8 h
-1
(4) hydrogen and polyalphaolefin mol ratio are 5-20;
The Ni/ nanometer Al of described loading type
2O
3Catalyzer, its carrier are the nanometer gama-alumina, and metallic nickel is catalytic active component; Wherein the charge capacity of metallic nickel is 1wt%-10wt%;
The Ni/ nanometer Al of described loading type
2O
3Catalyzer is by pickling process load nickelous nitrate, then by high temperature air roasting generation NiO/ nanometer Al at the alumina material with nano-scale particle
2O
3Catalyzer obtains Ni/ nanometer Al with hydrogen reducing before using
2O
3Catalyzer; Its concrete preparation process is as follows: according to the Ni/ nanometer Al of loading type
2O
3The content value of nickel takes by weighing nickelous nitrate in the catalyzer, uses dissolved in distilled water; Add nano aluminium oxide then, mix the back fully in ultrasonic machine ultrasonic 5-60 minute; At room temperature ventilation ageing 5-24h; 60-70 ℃ of following air seasoning, obtain dry mixture then, add thermal bake-out again in retort furnace, Heating temperature is 400-600 ℃, and roasting time is 1-10h; Before the use, catalyzer in the presence of hydrogen-nitrogen mixture gas, is reduced acquisition Ni/ nanometer Al in 200 ℃-500 ℃
2O
3Catalyzer; The volume content of hydrogen is 1%-100% in the described hydrogen-nitrogen mixture gas.
2. method according to claim 1 is characterized in that described polyalphaolefin, and molecular formula is C
nH
2n, wherein n is carbonatoms, is 20-100.
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|---|---|---|---|
| CN 201010574582 CN102079684B (en) | 2010-12-06 | 2010-12-06 | Method for catalyzing complete hydrogenation of polyalphaolefin into saturated alkane |
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|---|---|---|---|
| CN 201010574582 CN102079684B (en) | 2010-12-06 | 2010-12-06 | Method for catalyzing complete hydrogenation of polyalphaolefin into saturated alkane |
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|---|---|
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| CN102079684B true CN102079684B (en) | 2013-07-10 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304008A (en) * | 2011-06-13 | 2012-01-04 | 复旦大学 | Method for synthesizing saturated alkane by catalyzing poly-alpha olefin to be completely hydrogenated |
| CN102260133B (en) * | 2011-06-13 | 2013-10-16 | 复旦大学 | Complete hydrogenation method for synthesizing saturated alkane by catalyzing poly alpha olefin |
| RU2479562C1 (en) * | 2012-03-20 | 2013-04-20 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Волгоградский государственный технический университет" (ВогГТУ) | Method of producing straight-chain alkanes |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101890378A (en) * | 2009-05-19 | 2010-11-24 | 中国石油化工股份有限公司 | Hydrogenation catalyst and application thereof in residue fixed-bed hydrogenation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101890378A (en) * | 2009-05-19 | 2010-11-24 | 中国石油化工股份有限公司 | Hydrogenation catalyst and application thereof in residue fixed-bed hydrogenation method |
Non-Patent Citations (2)
| Title |
|---|
| 刘兴旺等.聚α-烯烃合成油的加氢改质.《石化技术》.2002,第9卷(第1期),第20页第2-3段，表4，第21页第1段，表6. |
| 聚α-烯烃合成油的加氢改质;刘兴旺等;《石化技术》;20021231;第9卷(第1期);第20页第2-3段，表4，第21页第1段，表6 * |
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