CN109030645A - A kind of method of carbon number distribution and n-alkane normal olefine in detection coal oil - Google Patents
A kind of method of carbon number distribution and n-alkane normal olefine in detection coal oil Download PDFInfo
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- CN109030645A CN109030645A CN201810803925.8A CN201810803925A CN109030645A CN 109030645 A CN109030645 A CN 109030645A CN 201810803925 A CN201810803925 A CN 201810803925A CN 109030645 A CN109030645 A CN 109030645A
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The method of carbon number distribution and n-alkane normal olefine in a kind of detection coal oil of the present invention；It is related to petroleum and tests and analyzes field；Using high temperature gas chromatography, using n-alkane, normal olefine after capillary chromatographic column, the appearance corresponding time on FID flame ionization ditector is different, measures the carbon number distribution of coal oil product and the content of n-alkane, normal olefine；Detection method of the present invention can be simple and quick completion in coal oil product coal light component oil, coal-to-olefin and coal system weight wax composition analysis, accuracy is high, practical, it is of great significance in terms of coal oil product testing, suitable for common lab to the testing requirements of product.
Description
Technical field
The present invention relates to petroleum to test and analyze field, and in particular to carbon number distribution and n-alkane in a kind of detection coal oil
The method of normal olefine.
Background technique
Coal oil be coal react at high temperature with oxygen, vapor, make coal all gasifications, be converted to carbon monoxide,
Then the mixture of methane and hydrogen synthesizes the technique skill of hydrocarbon under the action of iron-based or cobalt-base catalyst again
Art；Coal oil product is broadly divided into: coal-to-olefin, and boiling point is 50-350 DEG C, normal paraffin content 30-50%, normal olefine content
50-70%；Coal light component oil, 30-200 DEG C of boiling point, 95% or more Determination of Alkane Content；Coal system weight wax, 300-500 DEG C of boiling point, alkane
95% or more content；Carbon number distribution is that oil product is mainly made of the alkane or alkene of different carbon atoms, and carbon number distribution represents oil product
Carbon number compositing range；
Gas chromatographic technique can be tested component and fixation a separated reason of complicated mixture in a short period of time
The reason of showing as dissolution between liquid, generating dissolution is that there are cohesive force, including directive force, dispersion force, induction forces
With hydrogen bond force etc..After sample enters vaporizing chamber, each component rapid vaporization is simultaneously carried by carrier gas along pillar flowing, due to being tested group
Motive power between fractionated molecule and fixer molecule, tested component is just dissolved in fixer, simultaneously because the heat of molecule
Movement, the molecule dissolved can return in gas phase again, with the continuous flowing of carrier gas, be tested component in fixer and carrier gas two-phase
The distribution for carrying out continuous several times, expands the fine difference of cohesive force between each component, separates mixture.
In the detection for coal oil, the detection method of use is complicated, and it is not high that testing result provides time-consuming and accuracy,
Detailed analysis cannot be carried out to each component in coal oil.So also falling behind relatively in the detection technique to coal oil.
Summary of the invention
Overcome the deficiencies in the prior art of the present invention, it is therefore an objective to which carbon number distribution and n-alkane in a kind of detection coal oil are provided
The method of normal olefine.The detection method can be simple and quick completion to the carbon number distribution and n-alkane of coal oil product,
The composition analysis of normal olefine content, accuracy are high, practical.In order to solve the above technical problems, skill of the present invention
Art scheme are as follows:
A kind of method of carbon number distribution and n-alkane normal olefine in detection coal oil is utilized using high temperature gas chromatography
N-alkane, normal olefine are after capillary chromatographic column, and the appearance corresponding time on FID flame ionization ditector is not
Together, the carbon number distribution of coal oil product and the content of n-alkane, normal olefine are measured.
The coal oil product includes coal light component oil, coal-to-olefin and coal system weight wax；For coal light component oil
Detection parameters are as follows: 200 DEG C of injector temperature, split ratio 50:1, the setting of the column temperature of capillary chromatographic column: 30 DEG C of initial value, protect
It holds 2 minutes, is then warming up to 35 DEG C with 5 DEG C/min, kept for 1 minute, be then warming up to 100 DEG C with 10 DEG C/min, kept for 2 points
Clock.
For the detection parameters of coal-to-olefin are as follows: 300 DEG C of injector temperature, the column temperature setting of capillary chromatographic column: initial
It 50 DEG C of value, is kept for 2 minutes, is then warming up to 300 DEG C with 10 DEG C/min, kept for 20 minutes.
For the detection parameters of coal system weight wax are as follows: 350 DEG C of injector temperature, capillary chromatographic column column temperature setting: initial value
It 60 DEG C, is kept for 2 minutes, is then warming up to 360 DEG C with 5 DEG C/min, kept for 80 minutes.
Preferably, the sample volume is 0.2 μ l.
Coal oil be coal react at high temperature with oxygen, vapor, make coal all gasifications, be converted to carbon monoxide,
Then the mixture of methane and hydrogen synthesizes the technique skill of hydrocarbon under the action of iron-based or cobalt-base catalyst again
Art；Coal oil product is broadly divided into: coal-to-olefin, and boiling point is 50-350 DEG C, normal paraffin content 30-50%, normal olefine content
50-70%；Coal light component oil, 30-200 DEG C of boiling point, 95% or more Determination of Alkane Content；Coal system weight wax, 300-500 DEG C of boiling point, alkane
95% or more content；Carbon number distribution is that oil product is mainly made of the alkane or alkene of different carbon atoms, and carbon number distribution represents oil product
Carbon number compositing range.
The present invention is a kind of method of carbon number distribution and n-alkane normal olefine content for detecting coal oil product, specifically
Be to be detected to the product after ICL for Indirect Coal Liquefaction.The detection scheme of use is, using high temperature gas chromatography, to utilize positive structure
After capillary chromatographic column, the appearance corresponding time on FID flame ionization ditector is different for alkane, normal olefine,
To which simple and quick completion is to the carbon number distribution and n-alkane of coal oil product, the composition analysis of normal olefine content.
Compared with prior art the invention has the following advantages:
The present invention provides a kind of method of carbon number distribution and n-alkane normal olefine content for detecting coal oil product, passes through gas
Phase chromatography, only changing instrument parameter can be detected the carbon number distribution and n-alkane normal olefine of different coal oil product components
The method of content.The detection method can be simple and quick completion in coal oil product coal light component oil, coal-to-olefin and
The composition analysis of coal system weight wax, accuracy is high, practical, is of great significance, is suitable in terms of coal oil product testing
Testing requirements of the common lab to product.
Specific embodiment
1) instrument prepares
Instrument: Agilent 7890B gas chromatograph is equipped with FID flame ionization ditector.
Instrument: Agilent 7693A autosampler.
Reagent: C4-C12 n-alkane standard sample, C5-C30 n-alkane standard sample；C10-C80 n-alkane mark
Quasi- sample.
Material: high pure nitrogen purity 99.99%, high-purity hydrogen purity 99.99%, aeroscope 99.99%.
Chromatographic column: Agilent DB-1HT high temperature capillary chromatographic column, long 30m, internal diameter 0.25mm, film thickness 0.10um.
High pure nitrogen is opened, 25 ml/min of flow is set.
High pure air is opened, 300 ml/min of flow is set.
High-purity hydrogen is opened, 30 ml/min of flow is set.
2 ml/min of chromatographic column carrier gas flux is set.
2) coal-to-olefin step (C5-C30) is detected
It is ready to instrument preparation process, it is arranged 300 DEG C of instrument injector temperature in computer chromatographic work station, split ratio 50:1.
Instrument detector temperature is arranged 300 DEG C.
Column temperature setting: it 50 DEG C of initial value, is kept for 2 minutes, is then warming up to 300 DEG C with 10 DEG C/min, kept for 10 minutes.
Sample introduction: sample is added in 2ml chromatography column feed materials bottle, puts to sample injector, and sample volume is arranged in computer chromatographic work station
0.2 microlitre, instrument starts automatic sampling.
Instrument is about 37 minutes when analyzing.
Chromatogram, and the C5-C30 n-alkane standard sample spectrogram analyzed by same step are recalled after to be analyzed
It is compared.
Carbon number distribution: comparison C5-C30 n-alkane standard sample spectrogram, it is different according to the appearance time of different carbon, it obtains
The carbon number distribution of coal-to-olefin.
Normal paraffin content: area normalization method, by taking 10 n-alkane of carbon as an example, C5-C30 n-alkane standard sample are used
C10 n-alkane appearance time is 4.7 minutes on product spectrogram, and on coal-to-olefin sample spectrogram, finding appearance time is 4.7 points
The chromatographic peak of clock or so, corresponding content are 2.127%, i.e., C10 normal paraffin content is in expression coal-to-olefin sample
2.127%。
Normal olefine content: since the alkene and boiling point of alkanes of same carbon number are close, appearance time on a column is also connect
Closely, generally with carbon number same carbon number alkane previous position appearance.Using area normalization method, it is with 10 alkene of carbon
, C10 appearance time is 4.7 minutes on C5-C30 n-alkane standard sample spectrogram, on coal-to-olefin sample spectrogram, is found
The chromatographic peak that appearance time is 4.7 minutes or so is C10, and 4.5 before C10 alkane minute are C10 alkene, corresponding to contain
Amount is 7.041%, i.e., C10 olefin(e) centent is 7.041% in expression coal-to-olefin sample.
3) coal coal light component oil heavy oil step (C4-C10) is detected
It is ready to instrument preparation process, it is arranged 200 DEG C of instrument injector temperature in computer chromatographic work station, split ratio 50:1.
Instrument detector temperature is arranged 250 DEG C.
Column temperature setting:, being kept for 2 minutes, be then warming up to 35 DEG C with 5 DEG C/min by 30 DEG C of initial value, is kept for 1 minute, then
100 DEG C are warming up to 10 DEG C/min, is kept for 2 minutes.
Sample introduction: sample is added in 2ml chromatography column feed materials bottle, puts to sample injector, and sample volume is arranged in computer chromatographic work station
0.2 microlitre, instrument starts automatic sampling.
Instrument is about 12.5 minutes when analyzing.
4) coal heavy oil step (C8-C45) is detected
It is ready to instrument preparation process, it is arranged 300 DEG C of instrument injector temperature in computer chromatographic work station, split ratio does not shunt.
Instrument detector temperature is arranged 300 DEG C.
Column temperature setting: it 50 DEG C of initial value, is kept for 2 minutes, is then warming up to 300 DEG C with 10 DEG C/min, kept for 20 minutes.
Sample introduction: sample is dissolved in carbon disulfide in right amount, is added in 2ml chromatography column feed materials bottle, is put to sample injector, in computer color
It composes work station and is arranged 0.2 microlitre of sample volume, instrument starts automatic sampling.
Instrument is about 47 minutes when analyzing.
5) detection coal system weight wax step (C10-C75)
It is ready to instrument preparation process, it is arranged 350 DEG C of instrument injector temperature in computer chromatographic work station, split ratio does not shunt.
Instrument detector temperature is arranged 400 DEG C.
Column temperature setting: it 60 DEG C of initial value, is kept for 2 minutes, is then warming up to 360 DEG C with 5 DEG C/min, kept for 80 minutes.
Sample introduction: sample is dissolved in carbon disulfide in right amount, is added in 2ml chromatography column feed materials bottle, is put to sample injector, in computer color
It composes work station and is arranged 0.2 microlitre of sample volume, instrument starts automatic sampling.
Instrument is about 142 minutes when analyzing.
The above content is combine specific preferred embodiment to the further description done of the present invention, and it cannot be said that
A specific embodiment of the invention is only limitted to this, for those of ordinary skill in the art to which the present invention belongs, is not taking off
Under the premise of from the present invention, several simple deduction or replace can also be made, all shall be regarded as belonging to the present invention by being submitted
Claims determine scope of patent protection.
Claims (2)
1. a kind of method of carbon number distribution and n-alkane normal olefine in detection coal oil, which is characterized in that use High Temperature Gas
Phase chromatography, using n-alkane, normal olefine after capillary chromatographic column, on FID flame ionization ditector
The appearance corresponding time is different, measures the carbon number distribution of coal oil product and the content of n-alkane, normal olefine；
The coal oil product includes coal light component oil, coal-to-olefin and coal system weight wax；For the inspection of coal light component oil
Survey parameter are as follows: 200 DEG C of injector temperature, split ratio 50:1, the column temperature setting of capillary chromatographic column: 30 DEG C of initial value, kept for 2 points
Then clock is warming up to 35 DEG C with 5 DEG C/min, kept for 1 minute, be then warming up to 100 DEG C with 10 DEG C/min, kept for 2 minutes；
For the detection parameters of coal-to-olefin are as follows: 300 DEG C of injector temperature, the column temperature setting of capillary chromatographic column: initial value 50
DEG C, it is kept for 2 minutes, is then warming up to 300 DEG C with 10 DEG C/min, kept for 20 minutes；
For the detection parameters of coal system weight wax are as follows: 350 DEG C of injector temperature, the setting of capillary chromatographic column column temperature: 60 DEG C of initial value,
It is kept for 2 minutes, is then warming up to 360 DEG C with 5 DEG C/min, kept for 80 minutes.
2. the method for carbon number distribution and n-alkane normal olefine in a kind of detection coal oil according to claim 1,
It is characterized in that, the sample volume is 0.2 μ l.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114965792A (en) * | 2022-06-14 | 2022-08-30 | 宁夏滨泽新能源科技有限公司 | Analysis method for rapidly detecting content of C4-C22 alkane |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114965792A (en) * | 2022-06-14 | 2022-08-30 | 宁夏滨泽新能源科技有限公司 | Analysis method for rapidly detecting content of C4-C22 alkane |
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Address after: 046100 Yuwu Town, Tunliu District, Changzhi City, Shanxi Province (east of Yuwu town government) Applicant after: Shanxi Lu'an carbon one chemical Co., Ltd Address before: 046100 Shanxi city of Changzhi province Tunliu County Yu Wu Zhen Applicant before: SHANXI LU'AN NAKE TANYI CHEMICAL CO., LTD. |
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Application publication date: 20181218 |