CN112525840B - Rapid identification method for petroleum asphalt source - Google Patents
Rapid identification method for petroleum asphalt source Download PDFInfo
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- CN112525840B CN112525840B CN202011335794.9A CN202011335794A CN112525840B CN 112525840 B CN112525840 B CN 112525840B CN 202011335794 A CN202011335794 A CN 202011335794A CN 112525840 B CN112525840 B CN 112525840B
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- asphalt
- marker
- organic metal
- metal
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/72—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using flame burners
Abstract
The invention discloses a rapid identification method of petroleum asphalt sources. The method changes the method for identifying the sources by means of the property differences of the asphalt adopted in the prior art into the method for manually adjusting the composition of the asphalt, and effectively avoids the influence caused by objective factors such as crude oil, refining process and the like through the addition of the trace markers. The method selects oil-soluble metal organic matters, has good compatibility with petroleum asphalt and is not easy to separate out; the detection speed is high, and the number of required samples is small.
Description
Technical Field
The invention relates to the field of petrochemical industry, in particular to a rapid identification method of petroleum asphalt sources.
Background
With the development of social economy, the demand for petroleum asphalt is increasing, and the demand for asphalt quality is also increasing. Tens of asphalt production enterprises in China use different crude oil properties when asphalt is produced by different enterprises, different production processes are adopted, and the produced asphalt has uneven quality. Therefore, it is very important to effectively identify different brands of asphalt. Currently, three methods are commonly used to identify the source of bitumen.
The first one is a macroscopic index method, namely, on the basis that certain brands of asphalt have certain special properties, macroscopic indexes such as softening point, ductility and the like of asphalt products are analyzed to conduct approximate resolution. And secondly, a component analysis method, namely separating asphalt into four components of asphaltene, colloid, aromatic component and saturation component by a solvent filtration method, and identifying according to different contents of the four components of different asphalt. And thirdly, a fingerprint identification method (such as CN108469424A, CN102507718A, CN104198429A and the like), namely analyzing all brands of asphalt standard samples by using modern instrument analysis methods such as infrared spectrum, gel chromatography and the like, storing the obtained analysis results or patterns into a database, and comparing the results of the samples to be detected with the results in the database when the identification is performed, so as to infer the brands of the asphalt.
The first method belongs to an empirical method, is effective only for asphalt with special individual indexes, has no universality and is difficult to popularize and apply. The second method requires a large number of four-component analysis tests to be performed, which brings about a large amount of work and errors that are difficult to ignore, and in fact, the four-component differences between different bitumens are not obvious. The third method, although improving accuracy, is currently the most commonly used authentication method, but has the disadvantages: firstly, the premise of the method is that the production raw materials and the process of all brands of asphalt are kept stable and unchanged, which is difficult to realize under the actual condition, and once a certain asphalt production enterprise changes the production raw materials or the process, the method is not applicable any more; secondly, regardless of the process, the fractions of asphalt in petroleum are similar, and the spectrograms of asphalt of different brands can be similar, which brings great difficulty to the identification process; finally, the flow channels of crude oil are becoming more and more clear, and asphalt produced by two enterprises with the same crude oil and the same refining means is difficult to distinguish by the method.
In summary, the prior art schemes have serious technical defects, and the source of asphalt cannot be accurately and effectively identified.
Disclosure of Invention
The invention aims to provide a rapid identification method of petroleum asphalt sources, which is simple to operate, has continuous and effective results and is not influenced by external factors.
The invention provides a rapid identification method of petroleum asphalt sources, which comprises the following steps:
1) Adding an organic metal marker in the process of producing petroleum asphalt to obtain an asphalt sample to be tested;
the types of the organic metal markers are not less than 3;
and the addition amount of the organometallic marker is selected to be at least 2 levels of addition amount;
and unique organic metal marker-additive combination is distributed to different asphalt production enterprises;
2) And (2) analyzing the metal content of each organic metal marker in the asphalt sample to be detected obtained in the step (1) by adopting an atomic absorption spectrometer, and comparing the analysis result with the combination of the metal markers and the addition amount to determine the asphalt source.
In step 1) of the above method, the organometallic marker is an organic oil-soluble compound containing at least one of the following metal elements: fe. Cu, mn, K, na, al;
the effective metal content is greater than 20ppm to 500ppm, and the effective metal content differs by more than 100ppm between grades.
The method further comprises the steps of: before the organometal marker is added in said step 1), a demetallizing agent is added in the electro-desalting unit of the atmospheric and vacuum distillation apparatus.
The demetallizing agent is at least one selected from acid, complexing agent and surfactant;
the acid is specifically selected from at least one of phosphoric acid, formic acid and citric acid.
The demetallization agent is demetallization agent KJ-FMT1, and can be purchased from Hunan Changling petrochemical technology development Co.
The dosage of the demetallizing agent is 10-100 mug added into each g of crude oil; specifically 50 μg.
The time for adding the organic metal marker in the step 1) is to add the organic metal marker into the asphalt obtained by refining.
The beneficial effects of the invention are as follows:
1. the method for identifying the sources by means of the property differences of the asphalt adopted in the prior art is changed into the method for manually adjusting the composition of the asphalt, and the influence caused by objective factors such as crude oil, refining process and the like is effectively avoided by adding the trace markers.
2. The crude oil contains trace metal elements, and the content of the metal elements in the asphalt crude oil is controlled below 5ppm by adding the demetallizing agent, so that the influence of background noise on a detection result is eliminated, and the detection accuracy is improved.
3. Only a trace amount of markers are needed to be added, so that the road performance of asphalt is not reduced.
4. The oil-soluble metal organic matter is selected, so that the compatibility with petroleum asphalt is good, and the petroleum asphalt is not easy to separate out.
5. The detection speed is high, and the number of required samples is small.
Detailed Description
The invention will be further illustrated with reference to the following specific examples, but the invention is not limited to the following examples. The methods are conventional methods unless otherwise specified. The starting materials are available from published commercial sources unless otherwise specified.
Example 1,
1. The metal markers are selected as follows.
2. 8 addition schemes are formed and distributed to 8 different production enterprises, and the method is specifically as follows:
in the electric desalting unit of the atmospheric and vacuum distillation device, commercial demetallizing agent produced by a compounding method is added, the model is KJ-FMT1, and the blending amount of KJ-FMT1 in crude oil is 50 mug/g, which is produced by Hunan Changling petrochemical technology development Co.
When asphalt is produced by different enterprises, metal markers with specific compositions are added and stirred uniformly.
After obtaining 3 groups of samples to be tested, sampling and carrying out atomic emission spectrum analysis by using Perkinelmer in the United states, wherein an ashing method is adopted in a sample pretreatment method, a flame method is adopted in an atomization technology, pure copper naphthenate, aluminum stearate and sodium dodecyl sulfate are used as standard samples, and quantitative analysis results of three elements Cu, al and Na are obtained by adopting wavelengths of 324.8nm, 309.3nm and 766.5nm respectively, and the results are as follows:
| element(s) | Sample 1 | Sample 2 | Sample 3 |
| Cu | 71ppm | 5ppm | 74ppm |
| Al | 136ppm | 2ppm | 32ppm |
| Na | 65ppm | 8ppm | 66ppm |
And according to the effective content of the metal elements, finding a distribution scheme closest to each sample, determining that the sample 1 is produced by an enterprise 3, determining that the sample 2 is produced by other enterprises except enterprises 1-8, and determining that the sample 3 is produced by the enterprise 1.
Claims (7)
1. A method for rapid identification of petroleum asphalt sources, comprising:
1) Adding an organic metal marker in the process of producing petroleum asphalt to obtain an asphalt sample to be tested;
the types of the organic metal markers are not less than 3;
and the addition amount of the organometallic marker is selected to be at least 2 levels of addition amount;
and unique organic metal marker-additive combination is distributed to different asphalt production enterprises;
in the step 1), the organometallic marker is an organic oil-soluble compound containing at least one of the following metal elements: fe. Cu, mn, K, na, al;
the effective metal content is more than 20ppm to 500ppm, and the difference of the effective metal content between the grades exceeds 100ppm;
before the organic metal marker is added in the step 1), a demetallizing agent is added in an electric desalting unit of an atmospheric and vacuum distillation device;
2) And (2) analyzing the metal content of each organic metal marker in the asphalt sample to be detected obtained in the step (1) by adopting an atomic absorption spectrometer, and comparing the analysis result with the combination of the metal markers and the addition amount to determine the asphalt source.
2. The method according to claim 1, characterized in that: the demetallizing agent is at least one selected from the group consisting of an acid, a complexing agent and a surfactant.
3. The method according to claim 2, characterized in that: the acid is at least one selected from phosphoric acid, formic acid and citric acid.
4. A method according to any one of claims 1-3, characterized in that: the demetallizing agent is demetallizing agent KJ-FMT1.
5. A method according to any one of claims 1-3, characterized in that: the amount of the demetallizing agent is 10-100 mug added into each g of crude oil.
6. The method according to claim 5, wherein: the amount of demetallizing agent was 50. Mu.g.
7. A method according to any one of claims 1-3, characterized in that: the time for adding the organic metal marker in the step 1) is to add the organic metal marker into the asphalt obtained by refining.
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| CN202011335794.9A CN112525840B (en) | 2020-11-25 | 2020-11-25 | Rapid identification method for petroleum asphalt source |
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| CN202011335794.9A CN112525840B (en) | 2020-11-25 | 2020-11-25 | Rapid identification method for petroleum asphalt source |
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| CN112525840B true CN112525840B (en) | 2023-07-25 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4977328A (en) * | 1989-03-02 | 1990-12-11 | U.S. Philips Corporation | Method of detecting a marker provided on a specimen |
| WO1994012874A1 (en) * | 1992-11-27 | 1994-06-09 | Bp Oil International Limited | Method of identifying liquid petroleum products |
| CN104204802A (en) * | 2012-03-22 | 2014-12-10 | 田中贵金属工业株式会社 | Immunochromatography detection method |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BRPI0609385A2 (en) * | 2005-05-10 | 2011-10-18 | Commw Scientifc And Ind Res Organisation E The Boeing Company | methods for marking and tracking an industrial process material, system, and portable luminescence reader |
| CN102564998A (en) * | 2012-02-16 | 2012-07-11 | 湖南省湘电试研技术有限公司 | Method for identifying performance of reclaimed insulating oil |
| CN107101961B (en) * | 2017-06-22 | 2019-10-11 | 甘肃省交通规划勘察设计院股份有限公司 | A kind of method of Trace Metals Contents in aas determination pitch |
| CN108398398A (en) * | 2018-02-12 | 2018-08-14 | 山西省交通科学研究院 | The method for identifying asphalt quality using decaying In situ ATR-FTIR standard spectrogram |
| US10768164B2 (en) * | 2018-10-30 | 2020-09-08 | Ganzu Province Transportation Planning, Survey & Design Institute Co., Ltd. | Method for fast detecting pavement asphalt and early warning based on infrared spectrum big data |
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- 2020-11-25 CN CN202011335794.9A patent/CN112525840B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4977328A (en) * | 1989-03-02 | 1990-12-11 | U.S. Philips Corporation | Method of detecting a marker provided on a specimen |
| WO1994012874A1 (en) * | 1992-11-27 | 1994-06-09 | Bp Oil International Limited | Method of identifying liquid petroleum products |
| CN104204802A (en) * | 2012-03-22 | 2014-12-10 | 田中贵金属工业株式会社 | Immunochromatography detection method |
Non-Patent Citations (1)
| Title |
|---|
| 热再生沥青混合料混溶程度的研究概况;王洋 等;《建筑材料》;全文 * |
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