CN117467468A - Column chromatography method for rapidly separating stan in crude oil - Google Patents
Column chromatography method for rapidly separating stan in crude oil Download PDFInfo
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- CN117467468A CN117467468A CN202311589920.7A CN202311589920A CN117467468A CN 117467468 A CN117467468 A CN 117467468A CN 202311589920 A CN202311589920 A CN 202311589920A CN 117467468 A CN117467468 A CN 117467468A
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- molecular sieve
- stanes
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- 239000010779 crude oil Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000004440 column chromatography Methods 0.000 title description 4
- 239000002808 molecular sieve Substances 0.000 claims abstract description 32
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 32
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 28
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000926 separation method Methods 0.000 claims abstract description 15
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004202 carbamide Substances 0.000 claims abstract description 14
- 239000003208 petroleum Substances 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 claims abstract description 7
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000000706 filtrate Substances 0.000 claims description 27
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 26
- 230000007935 neutral effect Effects 0.000 claims description 26
- -1 polytetrafluoroethylene Polymers 0.000 claims description 20
- 239000003153 chemical reaction reagent Substances 0.000 claims description 15
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 9
- 230000013011 mating Effects 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000010828 elution Methods 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000003213 activating effect Effects 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 9
- OIGNJSKKLXVSLS-VWUMJDOOSA-N prednisolone Chemical compound O=C1C=C[C@]2(C)[C@H]3[C@@H](O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 OIGNJSKKLXVSLS-VWUMJDOOSA-N 0.000 abstract description 9
- 150000001335 aliphatic alkanes Chemical class 0.000 abstract description 8
- 238000010668 complexation reaction Methods 0.000 abstract description 5
- 239000003480 eluent Substances 0.000 abstract description 5
- 239000007790 solid phase Substances 0.000 abstract description 3
- 239000003463 adsorbent Substances 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000012046 mixed solvent Substances 0.000 abstract description 2
- ZRLNBWWGLOPJIC-PYQRSULMSA-N hopane Natural products C([C@]1(C)[C@H]2CC[C@H]34)CCC(C)(C)[C@@H]1CC[C@@]2(C)[C@]4(C)CC[C@@H]1[C@]3(C)CC[C@@H]1C(C)C ZRLNBWWGLOPJIC-PYQRSULMSA-N 0.000 description 9
- 238000010586 diagram Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- 238000001994 activation Methods 0.000 description 4
- 238000001819 mass spectrum Methods 0.000 description 4
- 150000002422 hopanes Chemical class 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 229930195734 saturated hydrocarbon Natural products 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000005526 G1 to G0 transition Effects 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 150000002391 heterocyclic compounds Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
- C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
- C10G53/08—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one sorption step
Landscapes
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention provides a method for rapidly separating stan in crude oil, which comprises the following steps: removing asphaltenes in the crude oil by adopting a centrifugal machine; eluting the stan-rich fraction from the crude oil with 1.5ml of a mixed solvent of 90% n-hexane and 10% petroleum ether; mixing urea and absolute ethyl alcohol with the fraction rich in sterane, adding n-hexane, and filtering to remove n-alkane; the 13X molecular sieve is used as a chromatographic column solid-phase adsorbent, and isooctane is used as eluent to purify the stane compound. The beneficial effects of the invention are as follows: the invention can rapidly separate asphaltene in crude oil by using a centrifuge, reduces the content of normal alkane in the fraction of the sterane by carrying out complexation reaction on the normal alkane and urea, and simultaneously further purifies the fraction of the sterane by using a 13X molecular sieve chromatographic column. Compared with the existing separation method, the method is simple and rapid, and the separated sterane has higher purity and stronger popularization and practical value.
Description
Technical Field
The invention belongs to the field of separation and purification of crude oil stane compounds, and particularly relates to a column chromatography method for rapidly separating stane in crude oil.
Background
The steroid compound is an important component part in saturated hydrocarbon, and has remarkable advantages in the aspects of exploring the source of crude oil matrix, characterizing the maturity of crude oil and the like by researching the content and ratio characteristics of the steroid compound. Meanwhile, the method has important geological and geochemical significance for the single hydrocarbon carbon isotopes. The separation methods of the stanes are mainly two, and the urea complexation method is reported in the literature to realize the purification of the stanes, but the content of the separated stanes is also pointed out to be low, and most samples are difficult to realize the effective separation of the stanes by the method except that some samples with extremely high stanes content can identify peaks. In addition, separation of the hopane compound can also be achieved by combining a plurality of molecular sieves of different pore sizes. However, the experimental procedures are complicated, the loss of the stane compound is serious, and the content of the enriched stane compound often cannot meet the requirement of a mass spectrum detection threshold value. Clearly, there is a need for a more rapid and efficient separation process for stanes in crude oil.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for rapidly separating sterane in crude oil. The method can remove normal alkane, residual hopane and other heterocyclic compounds in the fraction of the sterane to a great extent by using neutral alumina chromatographic column and urea complexation. The use of 13X molecular sieves as solid phase adsorbents may further purify the steroid compounds. The method comprises the following steps:
s1: measuring a preset amount of crude oil sample through a centrifuge tube, adding petroleum ether into the centrifuge tube, centrifuging the centrifuge tube through the centrifuge tube, and measuring filtrate on the top layer of the centrifuge tube to remove asphaltenes in the crude oil sample;
s2: respectively filling neutral alumina and 13X molecular sieve into different matched chromatographic devices after activation;
s3: adding the filtrate measured in the step S1 into the matched chromatographic device filled with neutral alumina in the step S2; eluting the filtrate in the matched chromatographic device by using an eluting reagent to obtain an eluted fraction; wherein the eluting reagent is a mixed solution of normal hexane and petroleum ether, and the eluting fraction is a fraction rich in stanes;
s4: adding urea and absolute ethyl alcohol into the elution fraction obtained in the step S3, fully mixing, adding n-hexane liquid, and filtering to obtain a filtering filtrate, wherein the filtering filtrate is the filtrate after removing n-alkane;
s5, adding the filtered filtrate obtained in the step S4 into the matched chromatographic device filled with the 13X molecular sieve in the step S2, and eluting the filtered filtrate in the matched chromatographic device through isooctane to obtain the high-purity stan.
Further, in the step S1, the working parameters of the centrifuge are as follows: the rotating speed is 4000r/min, and the centrifugal machine rotates for 5min.
Further, in the step S2, the matched chromatographic apparatus includes a pasteur pipette, a polytetrafluoroethylene tube and a small funnel.
Further, the matched chromatographic device filled with the neutral alumina is a first matched chromatographic device, the length of a Babbitt pipette of the first matched chromatographic device is 230mm, the aperture is 7mm, and 3g of neutral alumina is filled in the Babbitt pipette;
the length of the polytetrafluoroethylene tube of the first matched chromatographic device is 10mm, and the aperture of the polytetrafluoroethylene tube is 8mm;
the diameter of the small funnel of the first matched chromatographic device is 100mm, and the aperture of the bottom of the funnel is 7mm.
Further, in the step S5, the matched chromatographic device filled with the 13X molecular sieve is a second matched chromatographic device;
the length of a Pasteur pipette of the second matched chromatographic device is 300mm, the aperture of the Pasteur pipette is 7mm, and the Pasteur pipette is filled with 2g of 13X molecular sieve;
further, in the step S2, the particle size of the neutral alumina filled in the matched chromatographic device is 100-200 mu m, and in the step S3, the filtrate in the matched chromatographic device is eluted by 1.5mL of eluting reagent, wherein the eluting reagent comprises 90% of normal hexane and 10% of petroleum ether by mass; wherein the eluting speed of the eluting reagent test was 1mL/min.
Further, in the step S4, the mass of urea is 5g, the mass of absolute ethyl alcohol is 15ml, and the mass of n-hexane is 10ml.
Further, in the step S2, the particle size of the 13X molecular sieve filled in the chromatography device is 60 μm, and in the step S5, the chromatography device is eluted with 5mL isooctane.
Further, in the step S2, the activation process of the activated neutral alumina and the 13X molecular sieve is as follows: the neutral alumina and 13X molecular sieve activated sieve are placed in a muffle furnace at 450 ℃ for activation for 4 hours.
Further, in the step S1, the capacity of the centrifuge tube is 10mL, the weight of the crude oil sample measured by the centrifuge tube is 100mg, and the volume of petroleum ether added is 5mL.
The method for rapidly separating the stan in the crude oil has the beneficial effects that: the method comprises the following steps: petroleum ether is added into a crude oil sample, and the crude oil sample is centrifuged to obtain filtrate; different matched chromatographic devices are filled with neutral alumina and 13X molecular sieve; eluting the filtrate by eluting reagent, adding urea, absolute ethyl alcohol and normal hexane liquid into the eluted fraction, filtering to obtain filtered filtrate, and finally adding the filtered filtrate into a matched chromatographic device filled with a 13X molecular sieve, and eluting by isooctane to obtain high-purity stan. In the method, petroleum ether is added into a crude oil sample for centrifugal treatment, so that asphaltene in the crude oil can be rapidly removed; the neutral alumina filled mating chromatographic apparatus can remove most of the hopane and aromatic and non-hydrocarbon components in crude oil. Urea complexation can remove normal paraffins in the stan-rich fraction; the 13X molecular sieve filled matched chromatographic device can be used as a stationary phase to adsorb the hopane compound, thereby playing a role in purification. Compared with the original method, the method has better separation effect on the stane compound, higher experimental efficiency and stronger popularization and practical value.
Drawings
FIG. 1 TIC diagram (total ion flow diagram) of crude oil sample;
FIG. 2 is a partial magnified view of TIC (m/z 217 mass spectrum) of a crude oil sample;
FIG. 3 shows a TIC diagram of a stan-rich fraction with n-alkanes removed;
FIG. 4 is a partial magnified view of the normal alkane, rich stan fraction, stan TIC, removed;
FIG. 5 shows a TIC diagram of the isolated stane compound;
FIG. 6 shows an enlarged partial view of the TIC of the steroid compound isolated.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
Referring to fig. 1 to 6, the present embodiment provides a column chromatography method for rapidly separating stanoids in crude oil, comprising the following steps:
s1, taking a proper amount of crude oil sample from the centrifuge tube, adding petroleum ether, placing the crude oil sample into the centrifuge tube for rotation, and transferring out filtrate on the top layer of the centrifuge tube for later use. Wherein the capacity of the centrifuge tube is 10mL, the weight of the crude oil sample is 100mg, and the volume of petroleum ether added is 5mL.
Specifically, the asphaltenes were fully precipitated by placing the centrifuge tube into a 4000r/min centrifuge for 5min.
Referring to fig. 1 and 2, fig. 1 and 2 are respectively a total ion flow diagram and a mass spectrum diagram of a crude oil sample;
s2, placing neutral alumina and a 13X molecular sieve in an incubator at 450 ℃ for activation for 4 hours, and filling the mixture into a matched chromatographic column device. The adsorption of 100-200um neutral alumina to normal paraffins, stanes and hopanes in saturated hydrocarbons is different. In the process of eluting crude oil by using the mixed reagent, the first 0.5ml of eluent mainly contains normal alkane, 0.5-1.5 ml of eluent contains high-abundance stan, and 1.5-3 ml of eluent contains high-abundance hopane compound. By collecting the previous 1.5ml of eluent, most of the hopane compounds, aromatic hydrocarbons and non-hydrocarbon compounds in the crude oil can be removed. Urea complexation can completely remove normal paraffins in the stan-rich fraction. The 13X molecular sieve has strong adsorption effect on the hopane, and the hopane compounds in the fraction of the sterane with the normal alkane removed can be further removed by using the 13X molecular sieve as a solid-phase filler, so that the purity of the sterane is further improved. In the conventional operation, after neutral alumina and 13X molecular sieve are activated for 4 hours at 450 ℃ in a muffle furnace, the neutral alumina and 13X molecular sieve are required to be placed in a 120 ℃ incubator for constant temperature for 12 hours to be filled in a matched chromatographic device. In the embodiment, the activated neutral alumina and the 13X molecular sieve are directly filled into a matched chromatographic device, so that the separation effect of the steroid compound can be improved.
Specifically, the matched neutral alumina chromatographic device is formed by combining a Pasteur pipette, a polytetrafluoroethylene tube and a small funnel. Wherein the length of the Babbitt pipette is 230mm, the pore diameter of the Babbitt pipette is 7mm, and the Babbitt pipette is filled with 3g of neutral alumina. The length of the polytetrafluoroethylene tube is 10mm, and the aperture of the polytetrafluoroethylene tube is 8mm. The diameter of the small funnel is 100mm, and the aperture of the bottom of the funnel is 7mm.
The length of the Babbitt pipette matched with the 13X molecular sieve chromatographic device is 300mm, and the aperture of the Babbitt pipette is 7mm.
S3, transferring the filtrate in the centrifuge tube to the upper end of a matched chromatographic device filled with neutral alumina, and eluting the stan-rich fraction in the crude oil by using a mixed reagent.
Specifically, the crude oil sample of the matched chromatographic device is leached to 1.4 times of the filling amount.
Neutral alumina filled in the matched chromatographic device has the particle size of 100-200 mu m, and the stane-rich fraction is eluted by 1.5mL of mixed reagent.
Preferably, the fraction of the sterane is separated by a mixed reagent, which is discharged at a rate of 1mL/min.
S4, adding urea and absolute ethyl alcohol into the elution fraction obtained in the step S3, fully mixing, filtering after normal hexane liquid is added, and obtaining a filtering filtrate, wherein the filtering filtrate is a filtrate after normal alkane is removed; the mass of urea used in the process was 5g, the mass of absolute ethanol was 15ml, and the mass of n-hexane was 10ml.
Specifically, the volume of absolute ethanol mixed with the stan-rich fraction was 1.5 times that of n-hexane used.
Referring to fig. 3 and 4, fig. 4 and 5 are respectively a TIC diagram and a TIC partial enlarged view of a fraction enriched in stanes except n-alkanes;
s5, eluting with 5mL of isooctane to obtain a high-purity stane (compound) fraction.
Specifically, the Babbitt pipette is filled with 2g of 13X molecular sieve; the particle size of the packed 13X molecular sieve was 60 μm. The 13X molecular sieve was dried for 10min before rinsing the steroid compound with the mixed reagent.
Referring to fig. 5 and 6, in order to verify the experimental effect of a method for rapidly separating stanes in crude oil provided by the present invention, the separated high-purity stane fraction was subjected to chromatographic-chromatographic detection. The total ion flow diagram (TIC) of the isolated high purity stanes was determined after step S5. As can be seen from the chromatogram, the peak type distribution of the steroid compound is clear and is comparable with the m/z217 mass spectrum.
In summary, the invention adopts a centrifuge to remove asphaltene in crude oil, uses a mixed solvent of 90 percent of normal hexane and 10 percent of petroleum ether to elute a stan-rich fraction, uses absolute ethyl alcohol, urea and the stan-rich fraction to mix, and filters to remove normal alkane after adding normal hexane; the 13X molecular sieve is used for purifying the stane compound, so that the separation effect of the stane compound is good, and the popularization value is high.
While the invention has been described with respect to the preferred embodiments, the scope of the invention is not limited thereto, and variations and alternatives will be apparent to those skilled in the art within the scope of the invention.
In this document, terms such as front, rear, upper, lower, etc. are defined with respect to the positions of the components in the drawings and with respect to each other, for clarity and convenience in expressing the technical solution. It should be understood that the use of such orientation terms should not limit the scope of the protection sought herein.
The embodiments described above and features of the embodiments herein may be combined with each other without conflict.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (10)
1. A method for rapidly separating stanes in crude oil, which is characterized in that: the method comprises the following steps:
s1: measuring a preset amount of crude oil sample through a centrifuge tube, adding petroleum ether into the centrifuge tube, centrifuging the centrifuge tube through the centrifuge tube, and measuring filtrate on the top layer of the centrifuge tube to remove asphaltenes in the crude oil sample;
s2: respectively filling neutral alumina and 13X molecular sieve into different matched chromatographic devices after activation;
s3: adding the filtrate measured in the step S1 into the matched chromatographic device filled with neutral alumina in the step S2; eluting the filtrate in the matched chromatographic device by using an eluting reagent to obtain an eluted fraction; wherein the eluting reagent is a mixed solution of normal hexane and petroleum ether, and the eluting fraction is a fraction rich in stanes;
s4: adding urea and absolute ethyl alcohol into the elution fraction obtained in the step S3, fully mixing, adding n-hexane liquid, and filtering to obtain a filtering filtrate, wherein the filtering filtrate is the filtrate after removing n-alkane;
s5, adding the filtered filtrate obtained in the step S4 into the matched chromatographic device filled with the 13X molecular sieve in the step S2, and eluting the filtered filtrate in the matched chromatographic device through isooctane to obtain the high-purity stan.
2. A method for rapid separation of stanes from crude oil according to claim 1, wherein in step S1, the centrifuge operating parameters are as follows: the rotating speed is 4000r/min, and the centrifugal machine rotates for 5min.
3. A method for rapid separation of stanes from crude oil according to claim 1, wherein in step S2, the mating chromatographic apparatus comprises a pasteur pipette, a polytetrafluoroethylene tube and a small funnel.
4. A method for rapid separation of stan from crude oil according to claim 3, wherein the matched chromatographic device filled with neutral alumina is a first matched chromatographic device, the length of a Babbitt pipette of the first matched chromatographic device is 230mm, the aperture is 7mm, and 3g of neutral alumina is filled in the Babbitt pipette;
the length of the polytetrafluoroethylene tube of the first matched chromatographic device is 10mm, and the aperture of the polytetrafluoroethylene tube is 8mm;
the diameter of the small funnel of the first matched chromatographic device is 100mm, and the aperture of the bottom of the funnel is 7mm.
5. A method for rapid separation of stanes in crude oil according to claim 3, wherein in step S5, the matched chromatographic device filled with 13X molecular sieve is a second matched chromatographic device;
the length of the Babbitt pipette of the second matched chromatographic device is 300mm, the pore diameter of the Babbitt pipette is 7mm, and the Babbitt pipette is filled with 2g of 13X molecular sieve.
6. A method for rapid separation of a steroid alkane from crude oil according to claim 1, characterised in that in step S2 the neutral alumina filled in the mating chromatographic apparatus has a particle size of 100-200 μm and in step S3 the filtrate in the mating chromatographic apparatus is eluted with 1.5mL of eluting reagent comprising 90% by mass of n-hexane and 10% by mass of petroleum ether; wherein the eluting speed of the eluting reagent test was 1mL/min.
7. The method for rapidly separating stanes from crude oil according to claim 1, wherein in the step S4, the mass of urea is 5g, the mass of absolute ethanol is 15ml, and the mass of n-hexane is 10ml.
8. The method for rapidly separating stanes from crude oil according to claim 1, wherein in the step S2, the particle size of the 13X molecular sieve filled in the mating chromatographic apparatus is 60 μm, and in the step S5, the mating chromatographic apparatus is eluted with 5mL of isooctane.
9. A method for rapid separation of stanes from crude oil according to claim 1, wherein in step S2, the process of activating neutral alumina and 13X molecular sieve is as follows: the neutral alumina and 13X molecular sieve activated sieve are placed in a muffle furnace at 450 ℃ for activation for 4 hours.
10. The method for rapidly separating stanes from crude oil according to claim 1, wherein in the step S1, the capacity of the centrifuge tube is 10mL, the weight of the crude oil sample measured by the centrifuge tube is 100mg, and the volume of petroleum ether added is 5mL.
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| CN202311589920.7A CN117467468A (en) | 2023-11-24 | 2023-11-24 | Column chromatography method for rapidly separating stan in crude oil |
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| CN202311589920.7A CN117467468A (en) | 2023-11-24 | 2023-11-24 | Column chromatography method for rapidly separating stan in crude oil |
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