CN102495020A - Method for determining coal pitch by utilizing infrared spectrogram of coal pitch - Google Patents
Method for determining coal pitch by utilizing infrared spectrogram of coal pitch Download PDFInfo
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- CN102495020A CN102495020A CN2011103895541A CN201110389554A CN102495020A CN 102495020 A CN102495020 A CN 102495020A CN 2011103895541 A CN2011103895541 A CN 2011103895541A CN 201110389554 A CN201110389554 A CN 201110389554A CN 102495020 A CN102495020 A CN 102495020A
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- coal
- infrared spectrogram
- tar pitch
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Abstract
The invention discloses a method for determining coal pitch by utilizing an infrared spectrogram of the coal pitch, which comprises steps of preparing pitch solution by using a pitch sample, obtaining the infrared spectrogram, analyzing curve characteristics of the infrared spectrogram of the pitch solution, and determining whether the pitch sample is the coal pitch by comparing the curve characteristics of the infrared spectrogram of the pitch solution with curve characteristics of the infrared spectrogram of the coal pitch. The curve characteristics of the know infrared spectrogram of the coal pitch are described according to the infrared spectrogram within a range of 4000-400cm-1 from high to low as follows: -OH at the free state vibrates in a stretching mode to generate an absorption peak above 3000cm-1; a moderate-strength absorption peak appears close to the position of 2850cm-1, and absorption peak is provided with a sharp peak shape and represents symmetrical stretching vibration of methylene-CH2-; a plurality of weak peaks appear within the range of 2000-1600cm-1, and the weak peaks represent frequency multiplication and group frequency absorption of vibration of =C-H; and a plurality of absorption peaks with different strength appear within the range of 1000-550cm-1, and the absorption peaks represent flexural vibration of =C-H on benzene rings. The method is simple in operation and accurate in determination result.
Description
Technical field
The invention belongs to the asphalt material analysis technical field, be specifically related to a kind of method of utilizing the infrared spectrogram mensuration coal-tar pitch of coal-tar pitch.
Background technology
The most frequently used asphalt material is petroleum bitumen and coal-tar pitch in the road construction, and because of the complicacy of pitch composition use pitch being analyzed is the relatively work of difficulty at present.In recent years, along with the improvement of analytical instrument and the progress of universal and application technology, infrared spectrum has received concern to a certain degree in the chemical structure analysis of pitch, become one of the most frequently used micro-analysis method.Infrared spectrum is meant that with wavelength or wave number be horizontal ordinate, is the spectrogram of resulting reflection infrared-ray of ordinate and matter interaction with intensity or other character with wavelength change.IR spectroscopy is an important means during organic compound structure is identified, at organic structural analysis, particularly the evaluation aspect of functional group has vital role.But existing research and using shows, and is very few about the infrared spectrum spectrogram data of coal-tar pitch, therefore, utilizes infrared spectrum that the assay method of coal-tar pitch is still waiting further to explore and research.
Summary of the invention
To defective that exists in the above-mentioned prior art or deficiency; The objective of the invention is to, a kind of method of utilizing the coal-tar pitch infrared spectrogram to measure coal-tar pitch is provided, this method is according to the distinctive characteristic of the infrared spectrogram of coal-tar pitch; Characteristic to the infrared spectrogram of the unknown asphalt sample that records compares; Thereby whether be coal-tar pitch, this method is simple to operate if measuring this asphalt sample, and it is accurate to measure the result.
In order to achieve the above object, the present invention adopts following technical solution:
A kind of method of utilizing the infrared spectrogram mensuration coal-tar pitch of coal-tar pitch is characterized in that, specifically comprises the steps:
The infrared spectrum of the cold primer-oil of step 2, determination step one obtains its infrared spectrogram;
Step 3, interpretation of result;
The curve of the infrared spectrogram of analysis cold primer-oil is at infrared spectrum 4000～400cm
-1Characteristic in the wave-number range is compared this characteristic with the curvilinear characteristic of known coal-tar pitch infrared spectrogram, if both are in full accord, judge that then said unknown asphalt sample is a coal-tar pitch, otherwise be not coal-tar pitch.The curvilinear characteristic of said known coal-tar pitch infrared spectrogram is according to infrared spectrum 4000～400cm
-1Be described below from high to low in the wave-number range:
1) 3500cm
-1More than: free state-OH stretching vibration generation absorption peak;
2) 2920cm
-1Near the absorption peak that a medium tenacity occurs, the peak type is sharp-pointed, is methylene-CH
2-antisymmetric stretching vibration;
3) 2850cm
-1Near the absorption peak that a medium tenacity occurs, the peak type is sharp-pointed, is methylene-CH
2-symmetrical stretching vibration;
4) 2000～1600cm
-1Between several weak peaks appear, be=frequency multiplication and the group of C-H vibration absorb frequently;
5) 1000～550cm
-1Between the absorption peak that some intensity do not wait appears, on the phenyl ring=flexural vibrations of C-H.
Further, said step 1 specifically comprises the steps:
1) with tool plug triangular flask 120 ℃ of oven dry in following 20 minutes in baking oven of wash clean, is cooled to room temperature.
2) take by weighing the good asphalt sample 1g of fusing, be accurate to behind the radix point the 4th when taking by weighing, using CS in the tool plug triangular flask of unknown asphalt sample after oven dry
2Dissolving is mixed with concentration and is 5% cold primer-oil.
Further, said step 2 specifically comprises the steps:
Using the digital display pipettor is that 5% cold primer-oil is filled with the KBr liquid cell of thickness as 0.1mm with mass concentration, at 4000cm
-1～500cm
-1Scan in the scope, measure its infrared spectrum, obtain the infrared spectrogram of cold primer-oil.
Beneficial effect of the present invention:
1, the theoretical analysis foundation is abundant, the experimental principle science, and the infared spectrum analysis is accurate.
2, accurately take by weighing pitch, test process is strict, handles accurately, and it is minimum that experimental error is dropped to.
3, the figure spectrum signature data standard as a reference of the infrared spectrum of coal-tar pitch is proposed.
4, the test specimen convenient sample making, test speed is fast, data processing is simple, analysis result advantage accurately.
Description of drawings
Fig. 1 is the infrared spectrum curve of the asphalt sample of embodiment 1 test gained.
Below in conjunction with accompanying drawing and embodiment the present invention is further explained.
Embodiment
Rationale of the present invention:
Through discovering, there are notable difference in the infrared spectrum of coal-tar pitch and petroleum bitumen, rock asphalt; Coal-tar pitch consist of various aromatic hydrocarbonses and derivant thereof, and organic group has corresponding absorption frequency to infrared spectrum, therefore available infrared spectrogram characterizes coal-tar pitch, the composition and the structure of reflection pitch.The inventor at first studies the composition structure of coal-tar pitch, finds out the main functional group of its composition structure of reflection in the coal-tar pitch; Analyze the infrared absorption spectrum of main functional group in the coal-tar pitch then; Obtain absorption peak characteristic that coal-tar pitch infrared spectrum collection of illustrative plates should possess and with the corresponding relation of functional group, disclosed the absorption peak characteristic that the coal-tar pitch infrared spectrum should possess; The concrete analysis process is following:
The composition structure analysis of A, coal-tar pitch
Coal-tar pitch is the potpourri of mainly being made up of the derivant of aromatic hydrocarbons and oxygen thereof, sulphur, nitrogen, and the element composition mainly is C, H, O, S, N.Similar with the analytical approach of petroleum bitumen, the composition of coal-tar pitch is divided into 3 components, 1) uncombined carbon (free carbon), be equivalent to the bituminous matter in the petroleum bitumen, particle is than big many of bituminous matter; 2) resin, animi resin are the solid crystals structures, also are similar to the bituminous matter in the petroleum bitumen, and barras is similar to the resin in the petroleum bitumen; 3) oil content mainly is made up of the unsaturated aromatic hydrocarbons of liquid.
The infrared signature frequency analysis of main group in B, the coal-tar pitch
The component of coal-tar pitch is mainly aromatics.Contain two keys in the aromatic hydrocarbons, but, vibration coupling takes place between the conjugated double bond owing to formed the conjugated pi system.Aromatic ring=CH vibrates at 3050cm
-1A more weak peak appears.The flexural vibrations of aromatic ring=CH appear at 900～650cm
-1Between.In the infrared spectrum of aromatic hydrocarbons at 2000～1660cm
-1Between several weak peaks can appear, this is=frequency multiplication and the group of CH vibration absorb frequently.The C-H antisymmetric stretching vibration on the phenyl ring and the vibration of phenyl ring skeleton and frequency are at 3070～3030cm
-1The zone produces one group of absorption band; Its in-plane bending vibration bands of a spectrum are at 1300～1000cm
-1The place is prone to covered by other peaks; The out-of-plane bending vibration bands of a spectrum are at 900～650cm
-1The zone produces strong absorption peak, to confirming that benzene ring substitution group has characteristic.C-C skeletal vibration wave number is at 1250～1150cm
-1Unsaturated link C=C stretching vibration appears at 1660～1630cm
-1＞C=O stretching vibration district is 1900～1650cm
-1The district.Methylene-CH in the aliphatic hydrocarbon
2-the antisymmetric stretching vibration wave number be (2926 ± 10) cm
-1, the symmetrical stretching vibration wave number is (2853 ± 10) cm
-1C-C skeletal vibration wave number is at 1250～1150cm
-1
The infrared spectrogram spectrum signature of C, coal-tar pitch
By among A, the B coal-tar pitch being formed the analysis of structure and group infrared signature frequency, and the absorption peak characteristic that combines its spectral strength, inventor to summarize coal-tar pitch infrared spectrum curve to possess (strong and obviously be prone to the characteristic distinguished).This characteristic can judge exactly whether asphalt sample is coal-tar pitch.According to infrared spectrum 4000～400cm
-1Describe from high to low in the wave-number range, the absorption peak characteristic that coal-tar pitch (removing oil) infrared spectrum curve possesses is following:
1) 3500cm
-1More than: free state-OH stretching vibration generation absorption peak;
2) 2920cm
-1Near the absorption peak that a medium tenacity occurs, the peak type is sharp-pointed, is methylene-CH
2-antisymmetric stretching vibration;
3) 2850cm
-1Near the absorption peak that a medium tenacity occurs, the peak type is sharp-pointed, is methylene-CH
2-symmetrical stretching vibration;
4) 2000～1600cm
-1Between several weak peaks appear, be=frequency multiplication and the group of C-H vibration absorb frequently;
5) 1000～550cm
-1Between the absorption peak that some intensity do not wait appears, on the phenyl ring=flexural vibrations of C-H.
The method of utilizing the infrared spectrogram mensuration coal-tar pitch of coal-tar pitch of the present invention specifically comprises the steps:
1) with tool plug triangular flask 120 ℃ of oven dry in following 20 minutes in baking oven of wash clean, is cooled to room temperature.
2) take by weighing the good asphalt sample 1g of fusing, be accurate to behind the radix point the 4th when taking by weighing, using CS in the tool plug triangular flask of unknown asphalt sample after oven dry
2Dissolving is mixed with concentration and is 5% cold primer-oil.
The infrared spectrum of the cold primer-oil of step 2, determination step one obtains its infrared spectrogram;
1) using the digital display pipettor is that 5% cold primer-oil is filled with the KBr liquid cell of thickness as 0.1mm with mass concentration, at 4000cm
-1～500cm
-1Scan in the scope, measure its infrared spectrum, obtain the infrared spectrogram of cold primer-oil.
2) mensuration finishes, and uses CS
2Liquid cell is fully clean, liquid cell is dried subsequent use with infrared lamp.
Step 3, interpretation of result
The curve of the infrared spectrogram of analysis cold primer-oil is at infrared spectrum 4000～400cm
-1Characteristic in the wave-number range; This characteristic is compared with the curvilinear characteristic of known coal-tar pitch infrared spectrogram; If both are in full accord; Judge that then said unknown asphalt sample is a coal-tar pitch, otherwise be not coal-tar pitch that the curvilinear characteristic of said known coal-tar pitch infrared spectrogram is according to infrared spectrum 4000～400cm
-1Be described below from high to low in the wave-number range:
1) 3500cm
-1More than: free state-OH stretching vibration generation absorption peak;
2) 2920cm
-1Near the absorption peak that a medium tenacity occurs, the peak type is sharp-pointed, is methylene-CH
2-antisymmetric stretching vibration;
3) 2850cm
-1Near the absorption peak that a medium tenacity occurs, the peak type is sharp-pointed, is methylene-CH
2-symmetrical stretching vibration;
4) 2000～1600cm
-1Between several weak peaks appear, be=frequency multiplication and the group of C-H vibration absorb frequently;
5) 1000～550cm
-1Between the absorption peak that some intensity do not wait appears, on the phenyl ring=flexural vibrations of C-H.
Below verify the feasibility and the validity of method of the present invention through two concrete embodiment.
Embodiment 1:
Present embodiment is chosen No. 90 matrix coal-tar pitch of label and is carried out IR spectroscopy as unknown asphalt sample, and test apparatus of selecting for use and material have WQF-400 Fourier transformation infrared spectrometer, the fixed liquid cell of potassium bromide (thickness 0.1mm), electronic balance (100,000/precision), CS
2(analyzing pure) and digital display pipettor etc.
Tool plug triangular flask 120 ℃ of oven dry in following 20 minutes in baking oven with wash clean are cooled to room temperature; Take by weighing the good asphalt sample 1g of fusing with electronic balance, then with using CS in its tool plug triangular flask after oven dry
2Dissolving is mixed with concentration and is 5% cold primer-oil sample, is accurate to behind the radix point the 4th when taking by weighing; Using the digital display pipettor is that 5% cold primer-oil is filled with the KBr liquid cell of thickness as 0.1mm with mass concentration, at 4000cm
-1～500cm
-1Scan in the scope, measure its infrared spectrum, obtain the infrared spectrogram (referring to Fig. 1) of cold primer-oil; Mensuration finishes, and uses CS
2Liquid cell is fully clean, liquid cell is dried subsequent use with infrared lamp.
Analyze the infrared spectrum collection of illustrative plates of this unknown asphalt sample, its curve is at 3800～3600cm
-1, 2925cm
-1, 2850cm
-1, 2000～1600cm
-1, 650～910cm
-1There is the obvious characteristics absorption peak at the place, obtains the ft-ir characteristic absorption peak as shown in table 1 and the corresponding relation of group, is consistent with the coal-tar pitch diffuse reflectance infrared spectroscopy of theoretical analysis.Therefore, this asphalt sample of decidable is a coal-tar pitch, conforms to actual conditions.
The pitch ft-ir characteristic absorption peak of table 1 embodiment 1
| Absorption frequency, cm -1 | Corresponding group |
| 3800～3600 | Free state-the OH stretching vibration |
| 2925 | Methylene-CH 2-antisymmetric stretching vibration |
| 2850 | Methylene-CH
2- |
| 2000～1600 | The frequency multiplication of=C-H vibration absorbs with group frequently |
| 650～910 | The result of C-H wagging vibration on the phenyl ring |
| 2365～2335 | Fail all to deduct the CO in the air background during mapping 2And form |
Embodiment 2:
The unknown asphalt sample of present embodiment is chosen the matrix pitch of certain highway working-yard, obtains asphalt sample according to the method with embodiment 1 and measures infrared spectrogram; Analyze the infrared spectrum collection of illustrative plates of asphalt sample, its curve is at 3800～3600cm
-1, 2925cm
-1, 2850cm
-1, 2000～1600cm
-1, 650～910cm
-1There is the obvious characteristics absorption peak at the place, obtains the ft-ir characteristic absorption peak as shown in table 2 and the corresponding relation of group, is consistent with the coal-tar pitch diffuse reflectance infrared spectroscopy of theoretical analysis.Therefore, judge that this asphalt sample is a coal-tar pitch.Measure the back and confirm to construction party the feedback information of construction party has affirmed the unknown asphalt sample to be coal-tar pitch.
The pitch ft-ir characteristic absorption peak of table 2 embodiment 2
| Absorption frequency, cm -1 | Corresponding group |
| 3800～3600 | Free state-the OH stretching vibration |
| 2925 | Methylene-CH 2-antisymmetric stretching vibration |
| 2850 | Methylene-CH
2- |
| 2000～1600 | The frequency multiplication of=C-H vibration absorbs with group frequently |
| 650～910 | The result of C-H wagging vibration on the phenyl ring |
| 2365～2335 | Fail all to deduct the CO in the air background during mapping 2And form |
To sum up; The method of utilizing the infrared spectrogram mensuration coal-tar pitch of coal-tar pitch of the present invention, it is abundant that it measures theoretical foundation, accurately reflected the characteristic of coal-tar pitch infrared spectrum curve; And through the accurate test of asphalt sample having been obtained the infrared spectrum curve of asphalt sample; Through test of many times checking, that this method has is simple to operate, measure result's advantage accurately, overcome exist in the prior art because pitch is formed the defective of the complicated analysis difficulty that causes; Enriched and utilized theory and the time study achievement of infrared spectrum, can be widely used in the pitch analysis in the road construction the pitch qualitative analysis.
Claims (3)
1. a method of utilizing the infrared spectrogram mensuration coal-tar pitch of coal-tar pitch is characterized in that, specifically comprises the steps:
Step 1, the unknown asphalt sample that will choose are mixed with 5% cold primer-oil;
The infrared spectrum of the cold primer-oil of step 2, determination step one obtains its infrared spectrogram;
Step 3, interpretation of result;
The curve of the infrared spectrogram of analysis cold primer-oil is at infrared spectrum 4000～400cm
-1Characteristic in the wave-number range is compared this characteristic with the curvilinear characteristic of known coal-tar pitch infrared spectrogram, if both are in full accord, judge that then said unknown asphalt sample is a coal-tar pitch, otherwise be not coal-tar pitch; The curvilinear characteristic of said known coal-tar pitch infrared spectrogram is according to infrared spectrum 4000～400cm
-1Be described below from high to low in the wave-number range:
1) 3500cm
-1More than: free state-OH stretching vibration generation absorption peak;
2) 2920cm
-1Near the absorption peak that a medium tenacity occurs, the peak type is sharp-pointed, is methylene-CH
2-antisymmetric stretching vibration;
3) 2850cm
-1Near the absorption peak that a medium tenacity occurs, the peak type is sharp-pointed, is methylene-CH
2-symmetrical stretching vibration;
4) 2000～1600cm
-1Between several weak peaks appear, be=frequency multiplication and the group of C-H vibration absorb frequently;
5) 1000～550cm
-1Between the absorption peak that some intensity do not wait appears, on the phenyl ring=flexural vibrations of C-H.
2. the described method of utilizing the infrared spectrogram mensuration coal-tar pitch of coal-tar pitch of claim 1 is characterized in that said step 1 specifically comprises the steps:
1) with tool plug triangular flask 120 ℃ of oven dry in following 20 minutes in baking oven of wash clean, is cooled to room temperature.
2) take by weighing the good asphalt sample 1g of fusing, be accurate to behind the radix point the 4th when taking by weighing, using CS in the tool plug triangular flask of unknown asphalt sample after oven dry
2Dissolving is mixed with concentration and is 5% cold primer-oil.
3. the described method of utilizing the infrared spectrogram mensuration coal-tar pitch of coal-tar pitch of claim 1 is characterized in that said step 2 specifically comprises the steps:
Using the digital display pipettor is that 5% cold primer-oil is filled with the KBr liquid cell of thickness as 0.1mm with mass concentration, at 4000cm
-1～500cm
-1Scan in the scope, measure its infrared spectrum, obtain the infrared spectrogram of cold primer-oil.
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| CN2011103895541A CN102495020A (en) | 2011-11-30 | 2011-11-30 | Method for determining coal pitch by utilizing infrared spectrogram of coal pitch |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104198429A (en) * | 2014-09-12 | 2014-12-10 | 广西大学 | Method for analysis and differentiation of asphalt by combining infrared chromatography with gel permeation chromatography |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102033004A (en) * | 2009-09-30 | 2011-04-27 | 上海宝钢化工有限公司 | Preparation method of pitch microsection |
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2011
- 2011-11-30 CN CN2011103895541A patent/CN102495020A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102033004A (en) * | 2009-09-30 | 2011-04-27 | 上海宝钢化工有限公司 | Preparation method of pitch microsection |
Non-Patent Citations (3)
| Title |
|---|
| 周建石等: "煤焦油的分离和优质煤沥青的制备", 《河北师范大学学报/自然科学版》, vol. 35, no. 5, 30 September 2011 (2011-09-30) * |
| 沈益顺: "C/C复合材料浸渍用基体前驱体煤沥青的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》, no. 12, 15 December 2008 (2008-12-15), pages 020 - 41 * |
| 秦志宏 等: "两种烟煤CS2溶剂分次萃取物的FTIR分析", 《中国矿业大学学报》, vol. 34, no. 5, 30 September 2005 (2005-09-30) * |
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| CN104198429A (en) * | 2014-09-12 | 2014-12-10 | 广西大学 | Method for analysis and differentiation of asphalt by combining infrared chromatography with gel permeation chromatography |
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Application publication date: 20120613 |