CN113740271A - Detection method of quinoline insoluble substance - Google Patents
Detection method of quinoline insoluble substance Download PDFInfo
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- CN113740271A CN113740271A CN202010467026.2A CN202010467026A CN113740271A CN 113740271 A CN113740271 A CN 113740271A CN 202010467026 A CN202010467026 A CN 202010467026A CN 113740271 A CN113740271 A CN 113740271A
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- filter paper
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- quinoline
- test tube
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- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000001514 detection method Methods 0.000 title claims abstract description 9
- 239000000126 substance Substances 0.000 title abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000011088 calibration curve Methods 0.000 claims abstract description 10
- 238000012360 testing method Methods 0.000 claims description 23
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- 239000010426 asphalt Substances 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000003245 coal Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 239000011294 coal tar pitch Substances 0.000 abstract description 14
- 239000000295 fuel oil Substances 0.000 abstract description 13
- 239000003208 petroleum Substances 0.000 abstract description 13
- 239000002904 solvent Substances 0.000 description 13
- 239000011280 coal tar Substances 0.000 description 6
- 238000005259 measurement Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 239000011331 needle coke Substances 0.000 description 3
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000011300 coal pitch Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000006253 pitch coke Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a method for detecting quinoline insoluble substances (QI), which measures a colorimetric value of filter paper by using a colorimeter, and obtains a QI value corresponding to an L value according to a calibration curve prepared in advance, so that the concentration of quinoline insoluble substances in a sample can be accurately and quickly measured. The detection method is suitable for detecting the trace quinoline insoluble substances in various coal tar pitch and petroleum heavy oil components.
Description
Technical Field
The invention belongs to the field of chemical detection, and particularly relates to a rapid and accurate detection method of quinoline insoluble substances (QI).
Background
In the coking industry, coal tar recovered from crude gas generated by coal pyrolysis accounts for about 3-4% of charged coal, and the coal tar has very complex composition, and generally contains coke powder, coal slag, organic matters and fine solids obtained by polymerization of the coal tar, namely, so-called solvent insoluble matters. The solvent insoluble substances are mainly distributed in coal tar distillate or coal tar pitch obtained by distilling coal tar, and when the coal tar pitch is used as a raw material for producing pitch coke and needle coke, certain properties of the coke, such as Coefficient of Thermal Expansion (CTE) and Hardgrove Grindability Index (HGI), are influenced by the solvent insoluble substances.
Determination of quinoline insolubles is generally carried out according to GB/T2293-2008, with the following test procedures: adding quinoline into an asphalt sample, heating in a water bath, centrifuging, weighing dried double-layer filter paper, infiltrating with hot quinoline, pouring the centrifuged sample onto the filter paper for suction filtration, repeatedly filtering and washing with hot quinoline and hot toluene until the filtrate is not obviously yellow, taking out the filter paper, drying and weighing, and calculating the content of Quinoline Insoluble (QI).
In the GB/T2293-2008 standard, in order to calculate the amount of QI, it is necessary to take time to dry the filter paper and measure the mass of the filter paper to calculate the mass of the filter cake. However, in the production of needle coke using the coal tar product and the coal tar pitch product, it is necessary to measure the content according to Quinoline Insolubles (QI) in real time and to change the pretreatment operation conditions according to the test results as soon as possible. Therefore, a method is needed that allows for fast and simple measurements.
CN102607917A discloses a method for measuring high-content quinoline insolubles, which specifically comprises the following steps: 1) adding thermal quinoline into the residue in the centrifugal test tube after the sample is centrifuged, and dissolving by adopting an ultrasonic oscillation mode; 2) performing first centrifugal separation on the mixture in the centrifugal test tube in the step 1), and performing suction filtration on a dissolved substance in the centrifugal test tube; 3) adding hot quinoline into the insoluble substances in the centrifugal test tube after centrifugation in the step 2) for dissolution; 4) performing secondary centrifugal separation on the mixture in the centrifugal test tube in the step 3), and performing suction filtration on a dissolved substance in the centrifugal test tube; 5) and 4) transferring all residual insoluble substances in the centrifugal test tube after centrifugation in the step 4) to filter paper, washing and filtering the residual insoluble substances by using hot quinoline, toluene and acetone in sequence, and finally drying the filter paper to constant weight. This method is suitable for samples with high quinoline insolubles, but the measurement procedure and time taken is not reduced.
Disclosure of Invention
In view of the above problems in the prior art, it is an object of the present invention to provide a method for rapidly and accurately measuring the QI value of a product such as coal tar pitch, petroleum heavy oil, etc., especially in the case where the QI content of a sample is less than 0.1% by mass.
The detection method according to the invention comprises the following steps:
1. weighing 1g (weighed to 0.0001g) of the prepared asphalt sample, putting the coal asphalt sample into a 100ml beaker, putting the modified asphalt sample into a centrifugal test tube, and adding 25ml of quinoline (about 2/3 of the centrifugal test tube);
2. placing a beaker or a centrifugal test tube (placing the test tube into a beaker filled with water) containing a sample into a water bath kettle at 80 ℃, placing quinoline and toluene into the water bath kettle, stirring the sample if not needed, and taking out the sample after 30 min;
3. putting the modified asphalt sample into a centrifugal test tube, centrifuging for 20min at the rotation speed of 4000r/min, and taking out;
4. taking out the dried double-layer filter paper with the diameter of 125mm, placing the double-layer filter paper into a weighing bottle, placing the double-layer filter paper into a dryer, cooling for 20min, weighing, and reading the mass;
5. taking out the filter paper, paving the filter paper, clamping the filter paper by a clamp, and infiltrating the filter paper by hot quinoline;
6. starting a pump, uniformly stirring the centrifuged sample by using a glass rod, pouring the mixture onto filter paper for suction filtration, washing a beaker or a centrifugal test tube by using about 20ml of hot quinoline for several times, completely transferring the residues onto the filter paper, and washing the residues on the filter paper by using about 30ml of hot quinoline for several times;
7. after being pumped to be dry, pouring a proper amount of hot toluene for repeated filtration and washing until the filtrate has no obvious yellow color;
8. the colorimetric value (L value) of the filter paper was measured by a color difference meter, and a QI value corresponding to the L value was obtained from a calibration curve prepared in advance.
Preferably, the colorimeter is a konica minolta CR-400 colorimeter.
Drawings
Fig. 1 is a calibration curve showing the relationship between QI values and colorimetric values (L values) according to the detection method of the present invention.
Detailed Description
Hereinafter, the present invention will be described in detail. Before the description is made, it should be understood that the terms used in the present specification and the appended claims should not be construed as limited to general and dictionary meanings, but interpreted based on the meanings and concepts corresponding to technical aspects of the present invention on the basis of the principle that the inventor is allowed to define terms appropriately for the best explanation. Accordingly, the description proposed herein is just a preferable example for the purpose of illustrations only, not intended to limit the scope of the invention, so it should be understood that other equivalents and modifications could be made thereto without departing from the spirit and scope of the invention.
The inventors of the present invention found that a correlation exists between the chromaticity of the filter and the QI value in the sample by dissolving coal tar pitch and petroleum heavy oil in a solvent and passing the solution through the filter.
A solution obtained by mixing a solvent with coal tar pitch or petroleum heavy oil is filtered through a filter, and then the brightness L value of the filter paper of the filter is measured, and a calibration curve is obtained according to the known corresponding relation between the amount of the insoluble component in the solvent of the coal tar pitch or the petroleum heavy oil and the brightness L value. And measuring the brightness L value corresponding to the coal pitch or the petroleum heavy oil with unknown solvent insoluble components, and determining the content of the solvent insoluble substances in the coal pitch or the petroleum heavy oil according to the calibration curve to realize the quick and accurate measurement of the solvent insoluble substances.
Filtering coal tar pitch or petroleum heavy oil solutions with different QIs, measuring the L value of filter paper, performing QI measurement on the coal tar pitch or petroleum heavy oil solutions with different QIs in advance through GB/T2293-2008, correlating the brightness L of each sample with the value of the solvent insoluble component to obtain a calibration curve of the L value and insoluble substances of the coal tar pitch or petroleum heavy oil, and thus obtaining the rapid measurement method of the QI in the coal tar pitch or petroleum heavy oil based on the L value.
The calibration curve in the detection method is obtained by performing QI measurement on coal tar pitch or petroleum heavy oil solutions with different QIs through GB/T2293-2008 and correlating the colorimetric value L of each sample with the numerical value of quinoline insoluble substances.
When preparing the calibration curve, determining that the QI value of coal tar pitch or petroleum heavy oil is 1% (measured by GB/T2293-2008), then diluting with aromatic hydrocarbon solvent to obtain a sample with the QI content of 0.001-0.1%, then preparing according to the steps of 1-7 in GB/T2293-2008, taking out filter paper and measuring with a color difference meter. The corresponding L value of the sample with QI content of 0.011 percent is taken as 1, and the L values of other samples are correspondingly converted. Note that the aromatic hydrocarbon solvent used for dilution was also subjected to a brightness test in the same way as the sample preparation for correction of the test value of the sample.
The following examples are given by way of illustration of embodiments of the invention and are not to be construed as limiting the invention, and it will be understood by those skilled in the art that modifications may be made without departing from the spirit and scope of the invention. Unless otherwise specified, reagents and equipment used in the following examples are commercially available products.
Example 1
The method comprises the steps of obtaining refined asphalt by an asphalt pretreatment unit in the needle coke production process through a solvent precipitation method, wherein the QI of the refined asphalt is 0.04% and is used as a test sample 1, further removing the QI from the refined asphalt through a centrifugal process, obtaining samples 2, 3, 4 and 5 with different QI contents by controlling centrifugal force and centrifugal time, and operating No. 2-5 samples according to the steps 1-7 in GB/T2293-2008. The filter paper is then removed from the finished filter of step 7, tested for L value and the corresponding QI value is read through the calibration curve. Samples Nos. 1-5 were QI tested using the complete procedure of GB/T2293-2008.
Claims (2)
1. A method for detecting quinoline insolubles comprises the following steps:
1) weighing 1g (weighed to 0.0001g) of the prepared asphalt sample, putting the coal asphalt sample into a 100ml beaker, putting the modified asphalt sample into a centrifugal test tube, and adding 25ml of quinoline (about 2/3 of the centrifugal test tube);
2) placing a beaker or a centrifugal test tube (placing the test tube into a beaker filled with water) containing a sample into a water bath kettle at 80 ℃, placing quinoline and toluene into the water bath kettle, stirring the sample if not needed, and taking out the sample after 30 min;
3) putting the modified asphalt sample into a centrifugal test tube, centrifuging for 20min at the rotation speed of 4000r/min, and taking out;
4) taking out the dried double-layer filter paper with the diameter of 125mm, placing the double-layer filter paper into a weighing bottle, placing the double-layer filter paper into a dryer, cooling for 20min, weighing, and reading the mass;
5) taking out the filter paper, paving the filter paper, clamping the filter paper by a clamp, and infiltrating the filter paper by hot quinoline;
6) starting a pump, uniformly stirring the centrifuged sample by using a glass rod, pouring the mixture onto filter paper for suction filtration, washing a beaker or a centrifugal test tube by using about 20ml of hot quinoline for several times, completely transferring the residues onto the filter paper, and washing the residues on the filter paper by using about 30ml of hot quinoline for several times;
7) after being pumped to be dry, pouring a proper amount of hot toluene for repeated filtration and washing until the filtrate has no obvious yellow color;
8) the colorimetric value (L value) of the filter paper was measured by a color difference meter, and a QI value corresponding to the L value was obtained from a calibration curve prepared in advance.
2. The detection method according to claim 1, wherein the colorimeter in step 8) is a konica minolta CR-400 colorimeter.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010467026.2A CN113740271A (en) | 2020-05-28 | 2020-05-28 | Detection method of quinoline insoluble substance |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010467026.2A CN113740271A (en) | 2020-05-28 | 2020-05-28 | Detection method of quinoline insoluble substance |
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| CN113740271A true CN113740271A (en) | 2021-12-03 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101082588A (en) * | 2006-06-02 | 2007-12-05 | 汤新华 | Method for rapid detecting chemical fertillizers effective phosphorus content |
| CN102095724A (en) * | 2010-11-24 | 2011-06-15 | 青岛佳明测控仪器有限公司 | Method for determining copper content in water by biquinolyl spectrophotometry |
| CN102607917A (en) * | 2012-03-12 | 2012-07-25 | 中钢集团鞍山热能研究院有限公司 | Determination method for high-content quinoline insoluble |
| JP2014174011A (en) * | 2013-03-08 | 2014-09-22 | Jfe Chemical Corp | Method for measuring solvent insoluble matter in coal tar |
| CN110567852A (en) * | 2019-10-17 | 2019-12-13 | 北京旭阳科技有限公司 | Rapid detection method for quinoline insoluble substances in asphalt |
-
2020
- 2020-05-28 CN CN202010467026.2A patent/CN113740271A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101082588A (en) * | 2006-06-02 | 2007-12-05 | 汤新华 | Method for rapid detecting chemical fertillizers effective phosphorus content |
| CN102095724A (en) * | 2010-11-24 | 2011-06-15 | 青岛佳明测控仪器有限公司 | Method for determining copper content in water by biquinolyl spectrophotometry |
| CN102607917A (en) * | 2012-03-12 | 2012-07-25 | 中钢集团鞍山热能研究院有限公司 | Determination method for high-content quinoline insoluble |
| JP2014174011A (en) * | 2013-03-08 | 2014-09-22 | Jfe Chemical Corp | Method for measuring solvent insoluble matter in coal tar |
| CN110567852A (en) * | 2019-10-17 | 2019-12-13 | 北京旭阳科技有限公司 | Rapid detection method for quinoline insoluble substances in asphalt |
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