CN103105409A - Method for detecting free radical ration in coal tar - Google Patents
Method for detecting free radical ration in coal tar Download PDFInfo
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Abstract
The invention discloses a method for detecting free radical ration in coal tar. The method comprises the steps of removing moisture in the tar in a high speed centrifuging manner, and preserving a tar sample under low temperature or inert atmosphere; adopting a diamagnetism substance to deliquate DPPH(1,1-Diphenyl-2-picrylhydrazyl radical 2,2-Diphenyl-1-(2,4,6-trinitrophenyl) hydrazyl) to prepare a plurality of DPPH standard samples with different free radical concentrations, carrying out EPR (electron paramagnetic resonance) measurement, carrying out secondary integration on an EPR spectrogram, and recording the corresponding secondary integration area; establishing a standard curve according to the free radical contents of the DPPH standard sample with different free radical concentrations and the secondary integration area of the corresponding EPR spectrogram; and filling the tar sample into a pipe, measuring according to the same EPR measuring condition, carrying out secondary integration on the measured EPR spectrogram, and substituting the secondary integration area into the standard curve so as to obtain the free radical content N. The method provided by the invention can exactly measure free radical content in coal tar, meanwhile, the change of the content of the free radical in the coal tar along with the preservation condition is exactly measured, and the method for detecting ration is provided for the research of the free radical in the coal tar and is very simple and easy.
Description
Technical field
The present invention relates to a kind of method that free radical quantitatively detects, a kind of method that particularly in coal tar, free radical quantitatively detects.
Background technology
Coal is the main body energy of China, occupies for a long time 70% left and right of primary energy.The pyrolysis of coal refers to coal at isolated air or when continuous heating is to higher temperature under inert atmosphere conditions, and the series of physical that occurs changes and the complex process of chemical reaction.Pyrolysis of coal produces semicoke, tar, pyrolysis gas.Because petroleum resources are in short supply, pyrolysis of coal is produced carbocal tar and is day by day caused people's concern in recent years.Coalite tar refers to the tar that pyrolysis temperature produces when 600 ℃ and following temperature.It is a kind of industrial chemicals that high added value is arranged.The a large amount of paraffin that contain in coalite tar can separate by the method for freezing and filtering or extracting and use.The alternative sulfuric acid of the basic oil that contains in coalite tar is made Treatment of Metal Surface, and can further extract pyridine radicals.But neutral nitrogen compounds such as nitrile and derivant thereof obtain fatty amine through the hydrolysis obtain fatty acid after reduction.The liquefied olefines that contains in coalite tar, but cut obtains lubricating oil or makes washing agent through sulfonation.Heavy end can be made the asphalt oil of the use of building the road after chlorination, also can make light diesel and electrode coke through coking.Deacidify and except the cut after alkali, can obtain meeting by sequence of operations gasoline, diesel oil, the fuel wet goods product of petroleum products specification.
The problems such as existing pyrolytic technique ubiquity oil gas product yield is on the low side, pyrolysis oil studies on asphaltene content height.Therefore how to improve process conditions, improve hydrocarbon yield and become the task of top priority.Recent domestic recognizes that all the essence of pyrolysis of coal is free radical reaction course, and the weak covalent bond that originates in texture of coal dissociates, and comprises " secondary " reaction of generation, polymerization, restructuring, hydrogenation and these products of free radical.The core that improves simultaneously oil quality and productive rate is that the formation of coal free radical, transfer and stable orientation are controlled, and suppresses the free radical polycondensation and forms the bitum reaction of large molecule.By the rule of changes of free radicals in Study on Coal and pyrolysis product thereof, can form the response regulatory method of pyrolysis of coal free radical, realize the raising of hydrocarbon yield and quality.
Coal and char is the stable advantage that is beneficial to mensuration that waits of solid and free radical due to existence being arranged, and Chinese scholars is more to the research of its free-radical contents, and assay method is maturation comparatively also.Leslie R.Rudnick etc. are with 1 of concentration known, 1-diphenyl-2-picryl diazanyl (DPPH) ethanolic solution is standard model, tries to achieve number of free radical in coal liquefaction products by the method that compares the EPR spectrum quadratic integral area for the treatment of test sample and standard model under the same test condition.Qiu Nansheng etc. compose the number of free radical of the method calculating coal of quadratic integral area take solid-state DPPH as standard model by the EPR of sample and standard model under comparison same test condition.But above two kinds of methods are one-point method, forefathers existing solvent effect, standard specimen weighing error when using electronic paramagnetic resonance spectrometer (EPR) quantitative measurement free radical are large, the accuracy problem of one-point method in order to solve for Zheng Rongping etc., set up the calibration curve method of free radical in a kind of quantitative measurement coal, the method is dispersed in CaSO with solid DPPH
4In make the standard model of a series of concentration, Criterion curve.The method helps further long-term systematic research pyrolysis of coal mechanism and various factors on the impact of pyrolysis of coal process, also provides certain guidance for some other class sample EPR measure.Wu Aiping etc. utilize the method to observe the middle low-order coal in the different places of production at different temperatures (350-600 ℃), the situation of change of each parameter of free radical in the semicoke that produces in lower pyrolysis of coal process of the different residence time (0-30min), thereby the differentiation of free radical in the low-order coal pyrolytic process in research.
All below by the free radical in the solid product after coal and pyrolysis thereof being measured to explore the free radical reaction regulate and control method in the pyrolysis of coal process, to improve productive rate and the quality of tar.If the free-radical contents in energy direct-detection tar will help for the regulation and control of the free radical reaction in the pyrolysis of coal process provide more directly.
The context of detection of free radical in oil product, in Chinese patent CN 102590257 A, the people such as Yang Haijun uses electronic paramagnetic resonance spectrometer to detect free radical in oil product, by comparing the variation tendency of the free base unit weight in alternating temperature front and back, determine whether in waste oil or oil product doped with waste oil.But it just carries out the sxemiquantitative sign by internal standard method to the free radical in sample, can not quantify the number of free radical in oil product.Tar is the black viscous liquid, because the pyrolytic reaction process is very fast, the free radical that produces in pyrolytic process can be attached to the surface of product liquid, these free radicals are captured hydrogen atom generation condensation reaction and are settled out along with the variation meeting of time from proximity structure, or mutually combine the macromolecular material of generation between free radical, thereby affect the quality of tar.But tar is carried out exist when free-radical contents is measured the dress sample difficult, contain a certain amount of moisture, free-radical contents is low and the characteristics such as unstable, so its free-radical contents research seldom, also there is no the relevant report of free radical quantivative approach in tar at present.Therefore setting up free radical method for quantitatively determining in the perfect tar of a cover is very necessary for the exploration of free radical reaction in the evaluation of tar quality and pyrolysis of coal process.
Summary of the invention
The object of the invention is to overcome tar that above-mentioned prior art exists measure the fashionable dress sample difficult, contain a certain amount of moisture, free-radical contents is low and the defective such as unstable, found out tar and measured front suitable preservation condition, a kind of method that in coal tar, free radical quantitatively detects is provided.
The objective of the invention is to be achieved through the following technical solutions:
The present invention relates to a kind of method that in coal tar, free radical quantitatively detects, comprise the steps:
The processing of A, tar sample: high speed centrifugation is removed the moisture in tar;
The preservation of B, tar sample: preserve under low temperature or inert atmosphere;
The foundation of C, typical curve: adopt diamagnetic material dilution DPPH(1,1-diphenyl-2-trinitrophenyl-hydrazine), be mixed with some DPPH standard models of different number of free radical Ng; Described some DPPH standard models are carried out the EPR(electron paramagnetic resonance spectrum (EPR)) measure, the EPR spectrogram is carried out quadratic integral, the quadratic integral area A that record is corresponding; Quadratic integral area A Criterion curve according to the free-radical contents N of the DPPH standard model of different number of free radical Ng and corresponding EPR spectrum thereof;
D, tar sample tests: with the tar sample sample hose of packing into, measure according to measuring identical condition with EPR described in step C, the EPR spectrogram of the tar sample that records is carried out quadratic integral process, the described typical curve of quadratic integral area A substitution of gained is obtained free-radical contents N.
Preferably, in steps A, described ultracentrifugal centrifugal speed is higher than 8000r/min.
Preferably, in step B, described low temperature is lower than-40 ℃.
Preferably, in step C, described diamagnetic material is α-alundum (Al2O3), dead plaster or calcium carbonate.
Preferably, in step C, the condition that described EPR measures is: probe temperature 297K, microwave frequency 9.8 ± 10
-8GHz, microwave power 2.01～20.10mW measures number of times 1～10 time, central magnetic field 3510 ± 10
-6G, sweep length 100G, gain 1 * 10
2～1 * 10
4Time constant 1.25～163.84ms, sweep time 5.24～14.94s, modulating frequency 100kHz, modulation amplitude 0.5～2.0G.
Preferably, in step D, the described tar sample sample hose of packing into is specially: adopt the minute hand syringe directly the tar sample to be squeezed into the bottom of sample hose.
Preferably, with the substitution of free-radical contents N described in step D formula Ng=N/m, m refers to the quality of tar sample, namely gets number of free radical Ng.
Compared with prior art, the present invention has following beneficial effect:
1, by adjusting number of free radical and the consumption of standard specimen, the condition determination of optimizing simultaneously EPR has solved the few problem of free-radical contents in coal tar;
2, pass through temperature, before tar mensuration is found out in the exploration of the tar preservation conditions such as atmosphere, suitable preservation condition has solved the unsettled problem of free radical in tar;
3, can Accurate Determining go out the free-radical contents in coal tar, simultaneously can Accurate Determining coal tar in the content of free radical after changing with preservation condition; For the research of free radical in coal tar provides a kind of very simple and easy to do quantitative detecting method.
Description of drawings
By reading the detailed description of non-limiting example being done with reference to the following drawings, it is more obvious that other features, objects and advantages of the present invention will become:
Fig. 1 is the DPPH canonical plotting, and wherein N is the free-radical contents of DPPH standard model, and A is the quadratic integral area of the EPR spectrum of DPPH standard model.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.Following examples will help those skilled in the art further to understand the present invention, but not limit in any form the present invention.Should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make some distortion and improvement.These all belong to protection scope of the present invention.
Embodiment 1
The quantitative measurement of free radical in the Huainan coal pyrolytic tar.
1) processing of tar sample
The tar that produces after pyrolysis of coal is carried out high speed centrifugation, with upper strata tar and moisture from.
Contain a certain amount of moisture in tar, and water can absorb microwave, affect the mensuration of EPR, so the tar that pyrolysis of coal produces need to first be removed moisture, consider fast and can not destroy the factor of tar ingredients again, adopt high speed centrifugation (centrifugal speed is higher than 8000r/min) to remove fast the moisture in tar.
2) preservation of tar sample
Upper strata tar is preserved under nitrogen atmosphere, with to be determined.
Free radical in tar is unstable, can change along with the variation of holding time, and because the most of experimenter of the restriction of condition determination can not carry out the mensuration of EPR immediately after the tar output, so the preservation condition of tar seems most important.The present invention has investigated the impact of the factors such as temperature, preservation atmosphere on number of free radical in tar, finds the rising along with temperature, and the number of free radical rate of change is accelerated, and oxygen plays facilitation to the variation of number of free radical; So tar should preserve to reduce the variation of number of free radical under low temperature (lower than-40 ℃) or inert atmosphere before mensuration; Be chosen in the present embodiment under nitrogen atmosphere and preserve.
3) foundation of typical curve
Quantitatively take DPPH and CaSO
4, mixed grinding is even, and it is 1.221 * 10 that stepwise dilution is mixed with number of free radical Ng
18Spins/g, 0.611 * 10
18Spins/g, 0.458 * 10
18Spins/g, 0.305 * 10
18Spins/g, 0.153 * 10
18Spins/g, 0.076 * 10
18Spins/g, 0.038 * 10
18The DPPH standard model of spins/g, the DPPH standard model that takes each number of free radical of 10mg Ng carries out EPR and measures.
The EPR condition determination is: probe temperature 297K, microwave frequency 9.8 ± 10
-8GHz, microwave power 6.375mW measures number of times 6 times, central magnetic field 3510 ± 10
-6G, sweep length 90G, time constant 5.12ms, sweep time 20.97s, modulating frequency 100kHz, modulation amplitude 1G.
The EPR spectrogram is carried out quadratic integral, record its quadratic integral area.Carry out linear equation that linear regression obtains as N=5.67 * 10 take corresponding its EPR spectrum quadratic integral area of free-radical contents of the DPPH standard model of each number of free radical
6A+2.22 * 10
14
In formula, N is the free-radical contents of DPPH standard model, and A is the quadratic integral area of the EPR spectrum of DPPH standard model.Typical curve as shown in Figure 1, correlation coefficient r is 0.999, as shown in Figure 1, free-radical contents is 3.93 * 10
14～1.22 * 10
16Spins scope internal linear relation is good.
Typical curve set up process, be to adopt electronic paramagnetic resonance spectrometer to carry out EPR to the DPPH standard model of different number of free radical to measure.The free-radical contents that EPR is commonly used is measured standard specimen the Cr of mixing
3+Ruby crystals, raw coal, pitch, DPPH etc.Mix Cr
3+Ruby crystals be good standard specimen, but can not oneself the preparation, more be not easy to prepare the standard specimen of different spin concentrations (being number of free radical); Raw coal and pitch standard specimen spin population need first to demarcate with the standard specimen of known strength, and indirect calibration sample specified rate has brought inconvenience and accuracy is reduced; So the present invention adopts peak shape and goes out DPPH that the peak position all approaches with the pyrolysis of coal product as standard specimen, adopts diamagnetic material (α-Al
2O
3, dead plaster, calcium carbonate etc., select dead plaster in the present embodiment) dilution makes the standard specimen of different number of free radical Ng.
Because number of free radical in tar is lower, and the number of free radical of standard specimen can not unrestrictedly reduce, (optimal conditions is: probe temperature 297K, microwave frequency 9.8 ± 10 so need to be optimized the consumption of standard specimen and EPR condition determination (microwave power, modulation amplitude, mensuration number of times etc.)
-8GHz, microwave power 2.01～20.10mW measures number of times 1～10 time, central magnetic field 3510 ± 10
-6G, sweep length 100G, gain 1 * 10
2～1 * 10
4Time constant 1.25～163.84ms, sweep time 5.24～14.94s, modulating frequency 100kHz, modulation amplitude 0.5～2.0G) is then tested, and EPR spectrum (electron paramagnetic resonance spectrum (EPR)) is carried out quadratic integral process, and records its quadratic integral area.At last corresponding its EPR spectrum quadratic integral area of free-radical contents with the DPPH standard model of each number of free radical carries out the regression curve that linear regression obtains the suitable tar range of linearity.
4) the dress sample of tar sample
Get 101.7mg tar sample with the minute hand syringe and squeeze into paramagnetic pipe bottom.
Tar is the black viscous liquid, easily is stained with during sampling on the inwall of sample hose, is difficult to wiped clean, affects the accuracy of test result.Adopt the minute hand syringe directly sample to be squeezed into the bottom of sample hose, avoided above problem.
5) tar sample tests
Condition determination according to standard specimen is measured, and the EPR spectrogram of sample is carried out quadratic integral process, and quadratic integral area substitution typical curve is obtained free-radical contents N=1.4137 * 10
15Spins, number of free radical Ng=N/m=1.3901 * 10 in centrifugal rear tar
16Spins/g.
In sum, the present invention is by adjusting number of free radical and the consumption of standard specimen, and the condition determination of optimizing simultaneously EPR has solved the few problem of free-radical contents in coal tar; By to temperature, before the exploration of the tar preservation conditions such as atmosphere is found out tar and measured, suitable preservation condition has solved the unsettled problem of free radical in tar; Can Accurate Determining go out the free-radical contents in coal tar, simultaneously can Accurate Determining coal tar in the content of free radical after changing with preservation condition; For the research of free radical in coal tar provides a kind of very simple and easy to do quantitative detecting method.
Above specific embodiments of the invention are described.It will be appreciated that, the present invention is not limited to above-mentioned specific implementations, and those skilled in the art can make various distortion or modification within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (7)
1. the method that in a coal tar, free radical quantitatively detects is characterized in that, comprises the steps:
The processing of A, tar sample: high speed centrifugation is removed the moisture in tar;
The preservation of B, tar sample: preserve under low temperature or inert atmosphere;
The foundation of C, typical curve: adopt diamagnetic material dilution DPPH, be mixed with some DPPH standard models of different number of free radical; Described some DPPH standard models are carried out EPR measure, the EPR spectrogram is carried out quadratic integral, the quadratic integral area that record is corresponding; Quadratic integral area Criterion curve according to the free-radical contents of the DPPH standard model of different number of free radical and corresponding EPR spectrum thereof;
D, tar sample tests: with the tar sample sample hose of packing into, measure according to measuring identical condition with EPR described in step C, the EPR spectrogram of the tar sample that records is carried out quadratic integral process, the described typical curve of quadratic integral area substitution of gained is obtained free-radical contents.
2. the method that in coal tar according to claim 1, free radical quantitatively detects is characterized in that in steps A, described ultracentrifugal centrifugal speed is higher than 8000r/min.
3. the method that in coal tar according to claim 1, free radical quantitatively detects is characterized in that in step B, described low temperature is lower than-40 ℃.
4. the method that in coal tar according to claim 1, free radical quantitatively detects is characterized in that in step C, described diamagnetic material is α-alundum (Al2O3), dead plaster or calcium carbonate.
5. the method that in coal tar according to claim 1, free radical quantitatively detects is characterized in that, in step C, the condition that described EPR measures is: probe temperature 297K, microwave frequency 9.8 ± 10
-8GHz, microwave power 2.01～20.10mW measures number of times 1～10 time, central magnetic field 3510 ± 10
-6G, sweep length 100G, gain 1 * 10
2～1 * 10
4Time constant 1.25～163.84ms, sweep time 5.24～14.94s, modulating frequency 100kHz, modulation amplitude 0.5～2.0G.
6. the method that in coal tar according to claim 1, free radical quantitatively detects is characterized in that, in step D, the described tar sample sample hose of packing into is specially: adopt the minute hand syringe directly the tar sample to be squeezed into the bottom of sample hose.
7. the method that in coal tar according to claim 1, free radical quantitatively detects is characterized in that, with the substitution of free-radical contents N described in step D formula Ng=N/m, namely gets number of free radical Ng.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103472083A (en) * | 2013-09-17 | 2013-12-25 | 上海大学 | Method for detecting influence of electron beam irradiation on free radical concentration of coal by virtue of electron paramagnetic resonance |
| CN104502390A (en) * | 2014-12-12 | 2015-04-08 | 扬州大学 | Method for evaluating activation level of mechanical-chemical modified rubber powder |
| CN105021643A (en) * | 2014-04-18 | 2015-11-04 | 中国石油化工股份有限公司 | Method for measuring water contents of organic matters by virtue of nuclear magnetic resonance instrument |
| CN105628728A (en) * | 2015-12-24 | 2016-06-01 | 广州市市政工程设计研究总院 | Method for detecting change of concentration of hydroxyl radical in solution during reaction |
| CN106053513A (en) * | 2016-07-01 | 2016-10-26 | 江南大学 | Method for identifying adulterating gutter in refined vegetable oil |
| CN107219244A (en) * | 2017-06-12 | 2017-09-29 | 华东理工大学 | A kind of quantitative analysis method of utilization solid state nmr carbon spectrum detection texture of coal parameter |
| CN108508056A (en) * | 2018-02-05 | 2018-09-07 | 华中科技大学 | A kind of method of accurate quantification trace solid free-radical contents |
| CN110988009A (en) * | 2019-11-22 | 2020-04-10 | 浙江大学 | Pyrolysis reaction resonant cavity and EPR spectrometer |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103472083A (en) * | 2013-09-17 | 2013-12-25 | 上海大学 | Method for detecting influence of electron beam irradiation on free radical concentration of coal by virtue of electron paramagnetic resonance |
| CN103472083B (en) * | 2013-09-17 | 2016-01-20 | 上海大学 | A kind of method utilizing electron paramagnetic resonance detected electrons bundle irradiation to affect coal number of free radical |
| CN105021643A (en) * | 2014-04-18 | 2015-11-04 | 中国石油化工股份有限公司 | Method for measuring water contents of organic matters by virtue of nuclear magnetic resonance instrument |
| CN104502390A (en) * | 2014-12-12 | 2015-04-08 | 扬州大学 | Method for evaluating activation level of mechanical-chemical modified rubber powder |
| CN105628728A (en) * | 2015-12-24 | 2016-06-01 | 广州市市政工程设计研究总院 | Method for detecting change of concentration of hydroxyl radical in solution during reaction |
| CN106053513A (en) * | 2016-07-01 | 2016-10-26 | 江南大学 | Method for identifying adulterating gutter in refined vegetable oil |
| CN107219244A (en) * | 2017-06-12 | 2017-09-29 | 华东理工大学 | A kind of quantitative analysis method of utilization solid state nmr carbon spectrum detection texture of coal parameter |
| CN107219244B (en) * | 2017-06-12 | 2019-02-26 | 华东理工大学 | A kind of quantitative analysis method for composing detection texture of coal parameter using solid state nmr carbon |
| CN108508056A (en) * | 2018-02-05 | 2018-09-07 | 华中科技大学 | A kind of method of accurate quantification trace solid free-radical contents |
| CN110988009A (en) * | 2019-11-22 | 2020-04-10 | 浙江大学 | Pyrolysis reaction resonant cavity and EPR spectrometer |
| CN110988009B (en) * | 2019-11-22 | 2021-03-09 | 浙江大学 | Pyrolysis reaction resonant cavity for EPR spectrometer and EPR spectrometer |
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Inventor after: Pan Tieying Inventor after: Zhang Dexiang Inventor after: Wan Chuanling Inventor after: Yi Leqi Inventor after: Sun Changrong Inventor before: Pan Tieying Inventor before: Zhang Dexiang Inventor before: Wan Chuanling Inventor before: Yi Leqi |
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Application publication date: 20130515 |