CN102304008A - Method for synthesizing saturated alkane by catalyzing poly-alpha olefin to be completely hydrogenated - Google Patents
Method for synthesizing saturated alkane by catalyzing poly-alpha olefin to be completely hydrogenated Download PDFInfo
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- CN102304008A CN102304008A CN201110156870A CN201110156870A CN102304008A CN 102304008 A CN102304008 A CN 102304008A CN 201110156870 A CN201110156870 A CN 201110156870A CN 201110156870 A CN201110156870 A CN 201110156870A CN 102304008 A CN102304008 A CN 102304008A
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- polyalphaolefin
- poly
- alpha olefin
- hydrogen
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Abstract
The invention belongs to the technical field of fine chemical engineering and specifically relates to a method for synthesizing saturated alkane by catalyzing poly-alpha olefin to be completely hydrogenated. The method provided by the invention uses a deposition-precipitation method for hydrogenating Ni/Al2O3 catalyst. In the presence of Ni/Al2O3 catalyst, the poly-alpha olefin can be catalytically reduced to the saturated alkane under the conditions that the reaction temperature is in a range of 60-200 DEG C, the pressure range is 1.0-6.0 Mpa, the liquid hourly space velocity is 0.4-0.8 h<-1>, and the mol ratio of the hydrogen gas to the poly-alpha olefin is 5-20. The invention utilizes a simple and feasible method to realize that the poly-alpha olefin is completely hydrogenated and reduced to the alkane, so that an olefin double bond in the molecule is saturated, chemical stability and thermal stability of the product is ensured, and the conversion rate of the poly-alpha olefin can reach 100%. In the invention, a preparation process of the catalyst is simple and the cost is low. The method provided by the invention has a good application prospect.
Description
Technical field
The invention belongs to the fine chemical technology field, be specifically related to the method for the synthetic saturated alkane of the complete hydrogenation of a kind of catalysis 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 I. C. engine oil specification are strict more, many indexs only depend on mineral oil to be difficult to satisfy the requirement of new spec, impel the involutory olefiant interest of people to heighten, and have also promoted the demand growth of ucon oil in recent years.
The long-chain saturated alkane has been compared many advantages as the synthetic engine oil of base oil 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 this ucon oil and the oily price variance of mineral oil origin vehicular engine.
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, and lightning, point of ignition, spontaneous ignition temperature are high; 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, and efficient is high, and coking is few, nontoxic and skin had characteristics such as immersional wetting.
In the process of producing ucon oil, hope polyalphaolefin is carried out hydrogenation, make olefinic double bonds remaining in the molecule saturated, to guarantee the 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 pyritous steam turbine 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, coprecipitation method and the nickel-alumina catalyst of immersion process for preparing.Though adopt Raney's nickel can reach certain hydrogenation effect, Raney's nickel is instability in air, meet oxygen and burn easily, give to preserve and bring very big inconvenience with use.Though pickling process technology is simple, can practice thrift metal, but metal component is active relatively poor, and the short easy inactivation of life of catalyst, add precious metal after cost rise, be not suitable for present industrialization yet.Coprecipitation method is to obtain PAO hydrogenation one of preparation method preferably at present; And have satisfactory stability property, but the amount of the employed metal active constituent of this method is bigger, generally about 50wt.%; Increased the catalyzer cost virtually greatly, so in practical application, usually meet difficulty.
By comparison, adopt deposition-precipitation method to produce catalyzer and at first have the advantage of practicing thrift metallic nickel, and Al
2O
3Itself be exactly the common used in industry carrier, have the plurality of advantages that the strong raw material of the big inertia of surface-area extensively is easy to get.Therefore, the present invention provides a kind of active component nickel is dispersed in the method that obtains the big outside surface nickel catalyzator of high dispersive on the aluminum oxide, and is applied to the polyalphaolefin hydrogenation.
Summary of the invention
The method that the purpose of this invention is to provide the synthetic saturated alkane of the complete hydrogenation of catalysis polyalphaolefin that a kind of technology is simple, with low cost, efficient is high.
The method of the synthetic saturated alkane of the complete hydrogenation of polyalphaolefin provided by the invention, concrete steps are: the fixed bed that polyalphaolefin and hydrogen is together got into loading catalyst carries out catalyzed reaction, and polyalphaolefin is hydrogenated to alkane fully; Said catalyzer is synthetic through deposition-precipitation method by aluminum oxide and metallic nickel, is designated as Ni/Al
2O
3Catalyzer.Its reaction formula is:
C
nH
2n + H
2 → C
nH
2n+2 (n=20—100)。
The actual conditions of catalyzed reaction 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, described polyalphaolefin, molecular formula is C
nH
2n, wherein n is that carbonatoms is 20-100.
Among the present invention, said deposition-precipitation method synthesizes Ni/Al
2O
3The step of catalyzer is: the nitrate hydrate of metallic nickel is dissolved in an amount of water, then with active ingredient through deposition sedimentation to having on the fine grain alumina material; Through the high temperature air roasting, generate NiO/Al again
2O
3Before using, catalyzer, obtains Ni/Al with the reducing gas reduction
2O
3Catalyzer.Big, active high, the good stability of the catalyst surface area that the present invention makes.
Among the present invention, said Ni/Al
2O
3In the catalyzer, aluminum oxide (Al
2O
3) be the carrier of catalyzer, metallic nickel (Ni) is a catalytic active component.Wherein the charge capacity of metallic nickel is 5wt%-15wt%.
Among the present invention, the temperature of said high temperature air roasting is 400-600 ℃, and roasting time is 3-7 hours.
Among the present invention, said reducing gas is the mixed gas of hydrogen and nitrogen, and the content of hydrogen is 1%-100% in the reducing gas; Reduction temperature is 200-500 ℃.
The used deposition-precipitation method of the present invention synthesizes Ni/Al
2O
3The operation steps of catalyzer is following:
Certain density Al (the NO of preparation in the 500ml beaker
3)
3Solution, with ammoniacal liquor with Al (OH)
3Be precipitated out.Obtain Al (OH) with the B suction filtration
3After, respectively in 80 ℃, 120 ℃ baking ovens until its complete drying, place 600-700 ℃ of roasting 5--7h under the air atmosphere again, make aluminum oxide.Sieve after the aluminum oxide that makes ground, getting granularity is that 100 orders are following.Take by weighing a certain amount of Ni (NO
3)
2 .6H
2O adds suitable quantity of water and makes abundant dissolving in the 500ml beaker.Be that the following aluminum oxide of 100 orders is dispersed in the solution again with granularity, under churned mechanically condition, dropwise drip NaOH solution, make the pH value of solution remain on 7.8-8.2, stir 2--4h then.After stirring finishes precipitated liquid poured into suction filtration in the sand core funnel, and, use washing with alcohol again, in ambient temperature overnight with distilled water wash number time.Put into 70 ℃ of baking ovens until its complete drying, place 400-600 ℃ of roasting 3-7h under the air atmosphere again.Obtain Ni/Al
2O
3Catalyzer.
The present invention uses simple method, realizes that the complete hydrogenating reduction of polyalphaolefin becomes alkane, makes the olefinic double bonds in the molecule saturated, and to guarantee the 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.The present invention has a good application prospect.
Embodiment
Further describe the present invention through instance below.
Embodiment 1
Ni (5%)/Al
2O
3Catalyzer prepares as follows:
Certain density Al (the NO of preparation in the 500ml beaker
3)
3Solution, with ammoniacal liquor with Al (OH)
3Be precipitated out.Obtain Al (OH) with the B suction filtration
3After, respectively in 80 ℃, 120 ℃ baking ovens until its complete drying, place air atmosphere to be burnt 6h for following 700 ℃ again.With make aluminum oxide sieve after grinding, get the following 24g of 100 orders.Take by weighing the Ni (NO of 6.26g
3)
2 .6H
2O adds suitable quantity of water and makes abundant dissolving in the 500ml beaker.Again the aluminum oxide below 100 orders is dispersed in the solution, under churned mechanically condition, dropwise drips NaOH solution, the pH value of solution is remained on about 8, stir 3h then.After stirring finishes precipitated liquid poured into suction filtration in the sand core funnel, and with distilled water wash 3 times, washing with alcohol 2 times is in ambient temperature overnight.Put into 70 ℃ of baking ovens until its complete drying, place air atmosphere to be burnt 7h for following 400 ℃ again.Obtain Ni (5%)/Al
2O
3Catalyzer.
Restrain Ni (the 5%)/Al that gets ready with 10
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, getting into 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 (8%)/Al
2O
3Catalyzer prepares as follows:
Certain density Al (the NO of preparation in the 500ml beaker
3)
3Solution, with ammoniacal liquor with Al (OH)
3Be precipitated out.Obtain Al (OH) with the B suction filtration
3After, respectively in 80 ℃, 120 ℃ baking ovens until its complete drying, place air atmosphere to be burnt 6h for following 700 ℃ again.Be worth aluminum oxide sieve after grinding, get the following 24g of 100 orders.Take by weighing the Ni (NO of 10.33g
3)
2 .6H
2O adds suitable quantity of water and makes wherein branch dissolving in the 500ml beaker.Make the 100 order aluminum oxide that make be dispersed in the solution again, under churned mechanically condition, dropwise drip NaOH solution, the pH value of solution is remained on about 8, stir 3h then.After stirring finishes precipitated liquid poured into suction filtration in the sand core funnel, and with distilled water wash 3 times, washing with alcohol 2 times is in ambient temperature overnight.Put into 70 ℃ of baking ovens until its complete drying, place air atmosphere to be burnt 6h for following 450 ℃ again.Obtain Ni (8%)/Al
2O
3Catalyzer.
Restrain Ni (the 8%)/Al that gets ready with 10
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, getting into 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 (10%)/Al
2O
3Catalyzer prepares as follows:
Certain density Al (the NO of preparation in the 500ml beaker
3)
3Solution, with ammoniacal liquor with Al (OH)
3Be precipitated out.Obtain Al (OH) with the B suction filtration
3After, respectively in 80 ℃, 120 ℃ baking ovens until its complete drying, place air atmosphere to be burnt 6h for following 700 ℃ again.Be worth aluminum oxide sieve after grinding, get the following 24g of 100 orders.Take by weighing the Ni (NO of 13.21g
3)
2 .6H
2O adds suitable quantity of water and makes wherein branch dissolving in the 500ml beaker.Make the 100 order aluminum oxide that make be dispersed in the solution again, under churned mechanically condition, dropwise drip NaOH solution, the pH value of solution is remained on about 8, stir 3h then.After stirring finishes precipitated liquid poured into suction filtration in the sand core funnel, and with distilled water wash 3 times, washing with alcohol 2 times is in ambient temperature overnight.Put into 70 ℃ of baking ovens until its complete drying, place air atmosphere to be burnt 5h for following 500 ℃ again.Obtain Ni (10%)/Al
2O
3Catalyzer.
Restrain Ni (the 10%)/Al that gets ready with 10
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, getting into 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 (13%)/Al
2O
3Catalyzer prepares as follows:
Certain density Al (the NO of preparation in the 500ml beaker
3)
3Solution, with ammoniacal liquor with Al (OH)
3Be precipitated out.Obtain Al (OH) with the B suction filtration
3After, respectively in 80 ℃, 120 ℃ baking ovens until its complete drying, place air atmosphere to be burnt 6h for following 700 ℃ again.Be worth aluminum oxide sieve after grinding, get the following 24g of 100 orders.Take by weighing the Ni (NO of 17.77g
3)
2 .6H
2O adds suitable quantity of water and makes wherein branch dissolving in the 500ml beaker.Make the 100 order aluminum oxide that make be dispersed in the solution again, under churned mechanically condition, dropwise drip NaOH solution, the pH value of solution is remained on about 8, stir 3h then.After stirring finishes precipitated liquid poured into suction filtration in the sand core funnel, and with distilled water wash 3 times, washing with alcohol 2 times is in ambient temperature overnight.Put into 70 ℃ of baking ovens until its complete drying, place air atmosphere to be burnt 4h for following 530 ℃ again.Obtain Ni (10%)/Al
2O
3Catalyzer.
Restrain Ni (the 10%)/Al that gets ready with 10
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, getting into 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%)/Al
2O
3Catalyzer prepares as follows:
Certain density Al (the NO of preparation in the 500ml beaker
3)
3Solution, with ammoniacal liquor with Al (OH)
3Be precipitated out.Obtain Al (OH) with the B suction filtration
3After, respectively in 80 ℃, 120 ℃ baking ovens until its complete drying, place air atmosphere to be burnt 6h for following 700 ℃ again.Be worth aluminum oxide sieve after grinding, get the following 24g of 100 orders.Take by weighing the Ni (NO of 20.98g
3)
2 .6H
2O adds suitable quantity of water and makes wherein branch dissolving in the 500ml beaker.Make the 100 order aluminum oxide that make be dispersed in the solution again, under churned mechanically condition, dropwise drip NaOH solution, the pH value of solution is remained on about 8, stir 3h then.After stirring finishes precipitated liquid poured into suction filtration in the sand core funnel, and with distilled water wash 3 times, washing with alcohol 2 times is in ambient temperature overnight.Put into 70 ℃ of baking ovens until its complete drying, place air atmosphere to be burnt 3h for following 600 ℃ again.Obtain Ni (15%)/Al
2O
3Catalyzer.
Restrain Ni (the 15%)/Al that gets ready with 10
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, getting into 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 (5)
1. the method for the synthetic saturated alkane of the complete hydrogenation of catalysis polyalphaolefin is characterized in that concrete steps are: the fixed bed that polyalphaolefin and hydrogen is together got into loading catalyst carries out catalyzed reaction, and polyalphaolefin is hydrogenated to alkane fully; Said catalyzer is synthetic through deposition-precipitation method by aluminum oxide and metallic nickel, is designated as Ni/Al
2O
3Catalyzer; Wherein, the condition of catalyzed reaction is:
(1) temperature of reaction is 60-200
oC;
(2) reaction pressure 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.
2. method according to claim 1 is characterized in that said deposition-precipitation method synthesizes Ni/Al
2O
3The step of catalyzer is: the nitrate hydrate of metallic nickel is dissolved in an amount of water, then with active ingredient through deposition sedimentation to having on the fine grain alumina material; Generate NiO/Al through the high temperature air roasting again
2O
3Before using, catalyzer obtains Ni/Al with the reducing gas reduction
2O
3Catalyzer.
3. method according to claim 2 is characterized in that said Ni/Al
2O
3In the catalyzer, aluminum oxide is the carrier of catalyzer, and metallic nickel is a catalytic active component, and the charge capacity of metallic nickel is 5wt%-15wt%.
4. according to the said method of claim 2, it is characterized in that said high temperature air maturing temperature is 400-600 ℃, roasting time is 3-7 hours.
5. method according to claim 2 is characterized in that said reducing gas is the mixed gas of hydrogen and nitrogen, and the content of hydrogen is 1%-100% in the reducing gas; Reduction temperature is 200-500 ℃.
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|---|---|---|---|
| CN201110156870A CN102304008A (en) | 2011-06-13 | 2011-06-13 | Method for synthesizing saturated alkane by catalyzing poly-alpha olefin to be completely hydrogenated |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110156870A CN102304008A (en) | 2011-06-13 | 2011-06-13 | Method for synthesizing saturated alkane by catalyzing poly-alpha olefin to be completely hydrogenated |
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| Publication Number | Publication Date |
|---|---|
| CN102304008A true CN102304008A (en) | 2012-01-04 |
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104399469A (en) * | 2014-12-05 | 2015-03-11 | 复旦大学 | Catalyst for catalyzing maleic anhydride and hydrogenating to prepare butanedioic anhydride under low temperature and low pressure and preparation method of catalyst |
| CN106540698A (en) * | 2016-09-07 | 2017-03-29 | 西北大学 | A kind of preparation method of the loading type nickel-based catalyst of chloronitrobenzene selective hydrogenation synthesis chloro aminobenzen |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079684A (en) * | 2010-12-06 | 2011-06-01 | 复旦大学 | Method for catalyzing complete hydrogenation of polyalphaolefin into saturated alkane |
-
2011
- 2011-06-13 CN CN201110156870A patent/CN102304008A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079684A (en) * | 2010-12-06 | 2011-06-01 | 复旦大学 | Method for catalyzing complete hydrogenation of polyalphaolefin into saturated alkane |
Non-Patent Citations (2)
| Title |
|---|
| A.GIL ET AL.: "Influence of the preparation method and the nature of the support on the stability of the nickel catalysts", 《APPLIED CATALYSIS A:GENERAL》, vol. 109, 31 December 1994 (1994-12-31) * |
| H.SCHAPER ET AL.: "Synthesis of thermostable nickel-alumina catalysts by deposition-precipitation", 《APPLIED CATALYSIS》, vol. 16, 31 December 1985 (1985-12-31) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104399469A (en) * | 2014-12-05 | 2015-03-11 | 复旦大学 | Catalyst for catalyzing maleic anhydride and hydrogenating to prepare butanedioic anhydride under low temperature and low pressure and preparation method of catalyst |
| CN106540698A (en) * | 2016-09-07 | 2017-03-29 | 西北大学 | A kind of preparation method of the loading type nickel-based catalyst of chloronitrobenzene selective hydrogenation synthesis chloro aminobenzen |
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Application publication date: 20120104 |