CN105152841A - Low-temperature-freezing magnetic separation method and device for long-chain alkene and long-chain alkane mixture - Google Patents
Low-temperature-freezing magnetic separation method and device for long-chain alkene and long-chain alkane mixture Download PDFInfo
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- CN105152841A CN105152841A CN201510617184.0A CN201510617184A CN105152841A CN 105152841 A CN105152841 A CN 105152841A CN 201510617184 A CN201510617184 A CN 201510617184A CN 105152841 A CN105152841 A CN 105152841A
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Abstract
The invention relates to a low-temperature-freezing magnetic separation method for a long-chain alkene and long-chain alkane mixture. According to the low-temperature-freezing magnetic separation method, solid-liquid separation is easy to achieve, and product purity can be improved. Magnetic powder is added into the mixture liquid containing long-chain alkene and long-chain alkane, then mixed liquid containing the magnetic powder is cooled to be lower than the melting point of long-chain alkane and higher than the melting point of long-chain alkene, the long-chain alkane component is separated out and attracted to the surface of the magnetic powder to form magnetic waxy solid, the magnetic waxy solid is separated from unfrozen long-chain alkene liquid under the action of an external magnetic field, and after the magnetic waxy solid is taken out, molten liquid is heated to obtain long-chain alkane. The rate of freezing crystallization can be increased, solid-liquid separation is quite easy, and the high-purity product can be obtained. The method and device can be suitable for alkene separation of crude oil products and cutting oil obtained through Fischer-Tropsch synthesis in the coal chemical industry and separation and purification of mixed oil containing long-chain alkene in the petrochemical industry.
Description
Technical field
The present invention relates to being separated of long-chain olefin and long chain alkane, specifically a kind of method of cryogenic freezing Magneto separate long-chain olefin and paraffins mixture and device.
Background technology
Long-chain olefin (or being called higher olefins) refers to, containing alkene more than 10 carbon atoms, be divided into end alkene (α-alkene) and internal olefin according to position of double bond difference more.Long-chain olefin can produce the products such as olefin interpolymers, lubricating oil, tensio-active agent, oil field chemical, is widely used in petrochemical complex, light industry, weaving, metallurgy and the industry such as medicine, agricultural chemicals.But the separation of the long-chain olefin/paraffins mixture of same carbon atoms number is the significant technology issues that petrochemical complex and Coal Chemical Industry face.Therefore, the separation of long-chain olefin/paraffins mixture is also the focus of domestic and international separation field research, and separation method comprises multiple methods such as adopting rectifying, complexometric extraction, Absorptive complex wave and membrane sepn.
US4132744 discloses a kind of liquid-alkane of liquid extraction method separation of C 6 ~ C20 and the method for alkene mixture, with the mixture of the short chain alcohol containing silver salt or cuprous salt and fatty alcohol polyethers for extraction agent, wherein polyether solvent is 1,2-glycol dimethyl ether, diglyme, triglyme or 1,2-diethoxyethane, short chain alcohol is methyl alcohol, ethanol or n-propyl alcohol, is uniformly mixed by extraction agent with containing the mixing oil of alkene, major part alkene is transferred to extraction phase, after extraction phase is separated with extracting phase, extraction phase is distilled, obtain higher degree olefin product.
CN103232313A discloses a kind of extraction separating method of alkane/olefin, and extraction agent is N-Methyl pyrrolidone, N-N-formyl morpholine N-, 1-Methylimidazole or gamma-butyrolactone, and extraction agent is 0.25,0.5,1.0 or 2.0 with the cumulative volume ratio of mixture to be separated.Fully mixing is contacted with the mixture of the to be separated of high-carbon alpha-olefin with extraction agent with the alkane of carbon number by containing, then stratification being separated, wherein high-carbon alpha-olefin enters extraction phase, enters extracting phase with carbon alkane, realizes the alkane of same carbon number and being separated of high-carbon α-alkene.
UOP US2015/0148577 discloses the isomeric olefine of separation of C 19 ~ C22 from paraffin, be that the X-type zeolite of 2.4 ~ 2.6 is for sorbent material with optimum silica alumina ratio, adsorption temp 120 DEG C ~ 180 DEG C, simulation moving-bed carrying out is adopted to be separated the mixture containing long-chain olefin, desorbing agent is the naphthenic hydrocarbon of C5 ~ C10, as hexanaphthene, methylcyclohexane, methylcyclopentane etc., obtain the long-chain olefin product that concentration is higher.
Except above-mentioned document, have outward and be manyly separated report about long-chain olefin and alkane.Because the boiling point of same carbochain alkene and alkane is close, the theoretical plate number that rectifying separation needs is more, reflux ratio is comparatively large, energy consumption is very high.Complexometric extraction is separated comparatively ripe with Absorptive complex wave for short chain olefin, but there is more technology barrier for separating of long-chain olefin.Membrane separation technique is used for long-chain olefin and alkane separation is in development, has longer distance apart from industrialization.Comparatively speaking, the fusing point difference of the alkene of same carbon atoms number and alkane is comparatively large, and the difference of its fusing point can be utilized to adopt the method for cryogenic freezing to realize being separated of alkene and alkane.
US1313275 discloses a kind of method of cold temperature subzero fractionation long-chain olefin, with acetone, mibk or petroleum naphtha etc. for solvent, solvent and closing containing the mixture oil of long-chain olefin and alkane, the long chain alkane that reduction temperature makes fusing point higher solidifies precipitation, adopt the olefin hydrocarbon molecules that acetone or mibk equal solvent washing removing sandwich again, solid-liquid separation is carried out to waxy solid, steams solvent in filtrate by air lift, obtain the alkene of higher degree.
Comparatively speaking, adopt cryogenic freezing be separated long-chain olefin and paraffins mixture have simple to operate, do not introduce impurity and the lower advantage of energy consumption.At present, cryogenic freezing Crystallization Separation adopts falling-film crystallizer and kettle type crystallization device mostly, through decrease temperature crystalline, sweating is purified, heat up the process such as to thaw again, and falling-film crystallizer mainly forms crystallization rete at tube wall, does not need solid-liquid separation, but very easily contain impurity in rete, although adopt intensification sweating, a small amount of impurity is discharged, because viscosity is larger with sweat form, major part impurity still sandwiches at crystallizing layer inner, reduces the purity of product.The advantage of kettle type crystallization device is in decrease temperature crystalline process, stirring makes liquidus temperature more even, shortcoming is difficult to form nucleus and waxy solid not easily solid-liquid separation, or change in the temperature of solid-liquid separation process, makes partial condensate again be melted into liquid.
Summary of the invention
The cryogenic freezing Magneto separate long-chain olefin that the technical problem to be solved in the present invention is to provide and a kind ofly easily realizes solid-liquid separation, can improve product purity and the method for paraffins mixture.
For solving above technical problem, the technical solution used in the present invention is: a kind of method of cryogenic freezing Magneto separate long-chain olefin and paraffins mixture, magnetic powder is joined in the mixture liquid containing long-chain olefin and long chain alkane, then the mixing liquid containing magnetic powder to be cooled to lower than long chain alkane fusing point and in temperature range higher than long-chain olefin fusing point, long chain alkane component is separated out and is adsorbed in magnetic powder surface and forms magnetic waxy solid, in additional the action of a magnetic field magnetic waxy solid and not freezing long-chain olefin liquid separation, the liquid after melting that heats up after taking out magnetic waxy solid is long chain alkane.The magnetic medium that Magneto separate goes out is reusable.Long-chain olefin and paraffins mixture refer to that carbonatoms is greater than alkene and the alkane of the identical carbochain of 10.
Meanwhile, the present invention also provides the device of a kind of cryogenic freezing Magneto separate long-chain olefin and paraffins mixture, and the principle of design of this device and using method have identical design with aforesaid separation method.
Described device comprises stirring mixer, cooling system and magnetic separation system three part,
---stirring mixer comprises a double-jacket and column-shaped barrel, and cylindrical shell upper end is provided with charging opening, and lower end is provided with leakage fluid dram, and cylindrical shell, built with the agitator by driven by motor, encloses chuck outside cylindrical shell, and chuck lower end is provided with fluid inlet, and chuck upper end is provided with liquid outlet;
---cooling system comprises high/low temperature circulation all-in-one machine and recycle pump, and recycle pump is connected with the chuck lower end fluid inlet of stirring mixer, and the liquid outlet of chuck upper end is connected with high/low temperature circulation all-in-one machine;
---magnetic separation system comprises externally-applied magnetic field, is arranged on the bottom of stirring mixer.
The mode carrying out being separated long-chain olefin and long chain alkane adopting said apparatus is: be added in stirring mixer by the mixing liquid and magnetic powder that contain long-chain olefin and long chain alkane, starter motor stirs, and makes magnetic powder be suspended in oil phase; Start cooling system, cooling agent enters through recycle pump from stirring mixer chuck fluid inlet and is full of chuck, turns back to cooling system through liquid outlet; When fluid temperature in stirring mixer reaches the temperature of setting, cooling system maintains keeping warm mode, the freezing precipitation of long chain alkane component the surface being adsorbed in magnetic powder forms magnetic waxy solid, insulation 2 ~ 10
h; Then being shifted near by externally-applied magnetic field is attached to bottom stirring mixer, in stirring mixer, magnetic waxy solid condenses bottom mixing tank, open the leakage fluid dram of stirring mixer, give off not freezing long-chain olefin liquid, after liquid emptying, take out magnetic waxy solid and the thawing that heats up, after melting, liquid is long chain alkane product.
As preferred technical scheme, magnetic powder of the present invention has superparamagnetism, is Fe
3o
4, γ-Fe
2o
3, CoFe
2o, NiFe
2o
4and BaFe
2o
4in any one.The magnetic powder of superparamagnetism has magnetic when there being foreign field, and after cancelling externally-applied magnetic field, remanent magnetism disappears very soon, and magnetic powder does not have magnetic and particle diameter is tiny, and gentle agitation is just in dispersion state in a liquid.
As preferred technical scheme, externally-applied magnetic field of the present invention adopts permanent magnet, is selected from any one in ndfeb magnet, samarium cobalt magnet, alnico magnet and ferrite magnet.
The present invention, by adding magnetic powder, in crystallisation process, makes homogeneous nucleation process be converted into nonhomogen-ous nucleation, greatly can promote the speed of freezing and crystallizing, crystallization precipitate is attached to magnetic medium surface, in additional magnetic field environment, very easily solid-liquid separation, can obtain highly purified product.Method of the present invention and device are applicable to the thick oil product of F-T synthesis and the separation of olefins of cutting oil in Coal Chemical Industry, and petrochemical complex is containing the isolation andpurification of long-chain olefin mixing oil.
Accompanying drawing explanation
Fig. 1 be Magneto separate reactor of the present invention structural representation.
In figure, 1 stirring mixer, 1-1 cylindrical shell, 1-2 motor, 1-3 charging opening, 1-4 leakage fluid dram, 1-5 liquid exit, 1-6 liquid inlet, 1-7 chuck, 1-8 agitator, 2 cooling systems, the low circulation all-in-one machine of 2-1 high temperature, 2-2 recycle pump, 3 magnetic separation systems, 3-1 externally-applied magnetic field, 3-2 riser, 3-3 handle, 3-4 base.
Embodiment
Embodiment 1
The structure of cryogenic freezing Magneto separate long-chain olefin and paraffins mixture device and using method.
As shown in Figure 1, this device comprises stirring mixer 1, cooling system 2 and magnetic separation system 3 three part, wherein, stirring mixer 1 comprises a double-jacket and column-shaped barrel 1-1, and cylindrical shell upper end is provided with charging opening 1-3, and lower end is provided with leakage fluid dram 1-4, cylindrical shell is built with the agitator 1-8 driven by motor 1-2, enclose chuck 1-7 outside cylindrical shell, chuck 1-7 lower end is provided with fluid inlet 1-6, and chuck 1-7 upper end is provided with liquid outlet 1-5; Cooling system 2 comprises high/low temperature circulation all-in-one machine 2-1 and recycle pump 2-2, and recycle pump 2-2 is connected with the chuck 1-7 lower end fluid inlet 1-6 of stirring mixer 1, and the liquid outlet 1-5 of chuck 1-7 upper end is connected with high/low temperature circulation all-in-one machine 2-1; Magnetic separation system 3 comprises externally-applied magnetic field 3-1, is arranged on the bottom of stirring mixer 1.Externally-applied magnetic field 3-1 adopts permanent magnet, can select any one in ndfeb magnet, samarium cobalt magnet, alnico magnet and ferrite magnet.Externally-applied magnetic field 3-1 is placed in one with on the riser 3-2 of handle 3-3, bottom riser 3-2
There is base 3-4.
During use, be added in stirring mixer 1 by the mixing liquid and magnetic powder that contain long-chain olefin and long chain alkane, starter motor 1-2 stirs, and makes magnetic powder be suspended in oil phase; Start cooling system 2, cooling agent enters through recycle pump 2-2 from stirring mixer chuck 1-7 fluid inlet 1-6 and is full of chuck 1-7, turns back to cooling system 2 through liquid outlet 1-5; When in stirring mixer 1, fluid temperature reaches the temperature of setting, the temperature of this setting is in the temperature range lower than long chain alkane fusing point and higher than long-chain olefin fusing point, cooling system 2 maintains keeping warm mode, the freezing precipitation of long chain alkane component the surface being adsorbed in magnetic powder forms magnetic waxy solid, insulation 2 ~ 10
h; Then turning handle 3-3 makes riser 3-2 rise externally-applied magnetic field 3-1 to shift near and be attached to bottom stirring mixer 1, in stirring mixer 1, magnetic waxy solid condenses bottom mixing tank, open the leakage fluid dram 1-4 of stirring mixer 1, give off not freezing long-chain olefin liquid, after liquid emptying, take out magnetic waxy solid and the thawing that heats up, after melting, liquid is long chain alkane product.
Embodiment 2
Be 10%(mass ratio by 10L olefin(e) centent) laurylene and dodecane mixture join stirring mixer, then add the NiFe of 1kg particle diameter 500nm
2o
4powder, starter motor, stirs and makes NiFe
2o
4powder is suspended in oil phase.Set cooling temperature as-20 DEG C of (notes: the fusing point of dodecane is as-9 DEG C, the fusing point of laurylene is-33 DEG C), start cooling system, make mixing liquid cooling in stirring mixer, cool to about-20 DEG C, insulation 3h, mixing speed is 50rpm, discharge after Magneto separate and collect liquid, obtaining the carbon laurylene product that content is 90%.Take out magnetic waxy solid, be placed into normal temperature thawing and obtain dodecane.
Embodiment 3
Being 50%(mass ratio by 10L olefin(e) centent) tridecylene and tridecane mixture join stirring mixer, then add the Fe of 2kg particle diameter 500nm
3o
4powder, starter motor, stirs and makes Fe
3o
4powder is suspended in oil phase.Set cooling temperature as-15 DEG C of (notes: the fusing point of tridecane is as-5 DEG C, the fusing point of tridecylene is-23 DEG C), start cooling system, make mixing liquid cooling in stirring mixer, cool to about-15 DEG C, insulation 5h, mixing speed is 60rpm, discharge after Magneto separate and collect liquid, obtaining the carbon laurylene product that content is 93%.Take out magnetic waxy solid, be placed into normal temperature thawing and obtain tridecane.
Embodiment 4
Being 70%(mass ratio by 20L olefin(e) centent) ten pentaenes and pentadecane mixture join stirring mixer, then add the Fe of 1kg particle diameter 500nm
3o
4powder, starter motor, stirs and makes Fe
3o
4powder is suspended in oil phase.Setting cooling temperature is 3 DEG C of (notes: the fusing point of pentadecane is 8 DEG C, the fusing point of ten pentaenes is-3 DEG C), start cooling system, make mixing liquid cooling in stirring mixer, cool to about 3 DEG C, insulation 5h, mixing speed is 40rpm, discharge after Magneto separate and collect liquid, obtaining the carbon ten pentaene product that content is 92%.Take out magnetic waxy solid, be placed into normal temperature thawing and obtain pentadecane.
Embodiment 5
Being 30%(mass ratio by 10L olefin(e) centent) octadecylene and octadecane mixture join stirring mixer, then add the γ-Fe of 2kg particle diameter 400nm
2o
3powder, starter motor, stirs and makes γ-Fe
2o
3powder is suspended in oil phase.Setting cooling temperature is 20 DEG C of (notes: the fusing point of octadecane is 28 DEG C, the fusing point of octadecylene is 17 DEG C), start cooling system, make mixing liquid cooling in stirring mixer, cool to about 3 DEG C, insulation 4h, mixing speed is 60rpm, discharge after Magneto separate and collect liquid, obtaining the carbon octadecylene product that content is 90%.Take out magnetic waxy solid, be placed into normal temperature thawing and obtain octadecane.
Embodiment 6
Being 70%(mass ratio by 20L olefin(e) centent) ten pentaenes and pentadecane mixture join stirring mixer, then add the CoFe of 1kg particle diameter 500nm
2o4 powder, starter motor, stirs and makes CoFe
2o4 powder is suspended in oil phase.Setting cooling temperature is 3 DEG C of (notes: the fusing point of pentadecane is 8 DEG C, the fusing point of ten pentaenes is-3 DEG C), start cooling system, make mixing liquid cooling in stirring mixer, cool to about 3 DEG C, insulation 2h, mixing speed is 40rpm, discharge after Magneto separate and collect liquid, obtaining the carbon ten pentaene product that content is 92%.Take out magnetic waxy solid, be placed into normal temperature thawing and obtain pentadecane.
Embodiment 7
Being 50%(mass ratio by 10L olefin(e) centent) tridecylene and tridecane mixture join stirring mixer, then add the BaFe of 2kg particle diameter 500nm
2o
4powder, starter motor, stirs and makes BaFe
2o
4powder is suspended in oil phase.Set cooling temperature as-15 DEG C of (notes: the fusing point of tridecane is as-5 DEG C, the fusing point of tridecylene is-23 DEG C), start cooling system, make mixing liquid cooling in stirring mixer, cool to about-15 DEG C, insulation 10h, mixing speed is 60rpm, discharge after Magneto separate and collect liquid, obtaining the carbon tridecylene product that content is 93%.Take out magnetic waxy solid, be placed into normal temperature thawing and obtain tridecane.
Claims (6)
1. the method for a cryogenic freezing Magneto separate long-chain olefin and paraffins mixture, it is characterized in that: magnetic powder is joined in the mixture liquid containing long-chain olefin and long chain alkane, then the mixing liquid containing magnetic powder to be cooled to lower than long chain alkane fusing point and in temperature range higher than long-chain olefin fusing point, long chain alkane component is separated out and is adsorbed in magnetic powder surface and forms magnetic waxy solid, in additional the action of a magnetic field magnetic waxy solid and not freezing long-chain olefin liquid separation, the liquid after melting that heats up after taking out magnetic waxy solid is long chain alkane.
2. a device for cryogenic freezing Magneto separate long-chain olefin and paraffins mixture, is characterized in that: this device comprises stirring mixer (1), cooling system (2) and magnetic separation system (3) three part,
---stirring mixer (1) comprises a double-jacket and column-shaped barrel (1-1), cylindrical shell upper end is provided with charging opening (1-3), lower end is provided with leakage fluid dram (1-4), cylindrical shell is built with the agitator (1-8) driven by motor (1-2), chuck (1-7) is enclosed outside cylindrical shell, chuck (1-7) lower end is provided with fluid inlet (1-6), and chuck (1-7) upper end is provided with liquid outlet (1-5);
---cooling system (2) comprises high/low temperature circulation all-in-one machine (2-1) and recycle pump (2-2), recycle pump (2-2) is connected with chuck (1-7) lower end fluid inlet (1-6) of stirring mixer (1), and the liquid outlet (1-5) of chuck (1-7) upper end is connected with high/low temperature circulation all-in-one machine (2-1);
---magnetic separation system (3) comprises externally-applied magnetic field (3-1), is arranged on the bottom of stirring mixer (1).
3. utilize the method for device cryogenic freezing Magneto separate long-chain olefin and paraffins mixture described in claim 2, it is characterized in that: the mixing liquid and magnetic powder that contain long-chain olefin and long chain alkane are added in stirring mixer (1), starter motor (1-2) stirs, and makes magnetic powder be suspended in oil phase; Start cooling system (2), cooling agent to enter from stirring mixer chuck (1-7) fluid inlet (1-6) through recycle pump (2-2) and is full of chuck (1-7), turns back to cooling system (2) through liquid outlet (1-5); When in stirring mixer (1), fluid temperature reaches the temperature of setting, cooling system (2) maintains keeping warm mode, the freezing precipitation of long chain alkane component the surface being adsorbed in magnetic powder forms magnetic waxy solid, insulation 2 ~ 10
h; Then externally-applied magnetic field (3-1) is shifted near and be attached to stirring mixer (1) bottom, the interior magnetic waxy solid of stirring mixer (1) condenses bottom mixing tank, open the leakage fluid dram (1-4) of stirring mixer (1), give off not freezing long-chain olefin liquid, after liquid emptying, take out magnetic waxy solid and the thawing that heats up, after melting, liquid is long chain alkane product.
4. the method according to claim 1 or 3, is characterized in that: described magnetic powder has superparamagnetism, is Fe
3o
4, γ-Fe
2o
3, CoFe
2o, NiFe
2o
4and BaFe
2o
4in any one.
5. the method according to claim 1 or 3, is characterized in that: described externally-applied magnetic field adopts permanent magnet.
6. method according to claim 5, is characterized in that: described permanent magnet be selected from ndfeb magnet, samarium cobalt magnet, alnico magnet and ferrite magnet any one.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510617184.0A CN105152841B (en) | 2015-09-25 | 2015-09-25 | Freezing Magneto separate long-chain olefin and the method and device of paraffins mixture |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510617184.0A CN105152841B (en) | 2015-09-25 | 2015-09-25 | Freezing Magneto separate long-chain olefin and the method and device of paraffins mixture |
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| Publication Number | Publication Date |
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| CN105152841A true CN105152841A (en) | 2015-12-16 |
| CN105152841B CN105152841B (en) | 2017-03-01 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108949221A (en) * | 2018-07-17 | 2018-12-07 | 中国石油大学(华东) | A kind of magnetism dewaxing agent and magnetic process for dewaxing |
| CN109295490A (en) * | 2018-11-26 | 2019-02-01 | 镇江市高等专科学校 | A kind of Ni ferrite electrophoresis suspensioning liquid and its preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4132744A (en) * | 1977-12-12 | 1979-01-02 | Texaco Inc. | Process for separating liquid olefin-paraffin mixtures |
| CN103232313A (en) * | 2013-05-06 | 2013-08-07 | 北京化工大学 | Extraction and separation method of alkane/olefin |
| US20150148577A1 (en) * | 2013-11-26 | 2015-05-28 | Uop Llc | Separation of iso-olefins from paraffins in the c19 to c22 range |
-
2015
- 2015-09-25 CN CN201510617184.0A patent/CN105152841B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4132744A (en) * | 1977-12-12 | 1979-01-02 | Texaco Inc. | Process for separating liquid olefin-paraffin mixtures |
| CN103232313A (en) * | 2013-05-06 | 2013-08-07 | 北京化工大学 | Extraction and separation method of alkane/olefin |
| US20150148577A1 (en) * | 2013-11-26 | 2015-05-28 | Uop Llc | Separation of iso-olefins from paraffins in the c19 to c22 range |
Non-Patent Citations (1)
| Title |
|---|
| 邝生鲁 等: "烯烃/链烷烃分离工艺进展", 《现代化工》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108949221A (en) * | 2018-07-17 | 2018-12-07 | 中国石油大学(华东) | A kind of magnetism dewaxing agent and magnetic process for dewaxing |
| CN108949221B (en) * | 2018-07-17 | 2020-12-01 | 中国石油大学(华东) | Magnetic dewaxing agent and magnetic dewaxing method |
| CN109295490A (en) * | 2018-11-26 | 2019-02-01 | 镇江市高等专科学校 | A kind of Ni ferrite electrophoresis suspensioning liquid and its preparation method and application |
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|---|---|
| CN105152841B (en) | 2017-03-01 |
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