Method for determining quinoline insoluble in high-softening-point material

Abstract

The invention discloses a method for determining quinoline insoluble in a high-softening-point material, which comprises the following steps: S1, grinding the high-softening-point material into powder, taking 0.5-3 g of the powder as a sample, placing the sample in a beaker, pouring 10-15 ml of quinoline, placing the beaker on an electric furnace, and heating the beaker to a sample dissolving temperature; s2, after heating to the sample dissolving temperature, continuously heating to increase the temperature by 30-80 DEG C, stirring for 2-5 minutes, immediately transferring a feed liquid into a preheated sand star funnel, and carrying out suction filtration to obtain a filter cake; and S3, washing off quinoline remaining on the filter cake with cold toluene, then drying the sand star funnel and the filter cake, then transferring the sand star funnel and the filter cake into a dryer for cooling treatment, and then carrying out weighing calculation. According to the invention, the phenomenon of inaccurate analysis result caused by blockage of filter holes due to temperature drop in the suction filtration process can be avoided; the method has the advantages of being short in time consumption, fast in result obtaining, high in data accuracy and precision, good in reproducibility and the like.

Description

Technical Field

[0001] The invention belongs to the technical field of analysis and detection, and relates to a method for determining quinoline insoluble matter in high-softening point materials. The method is not only suitable for determining high-content quinoline insoluble matter in high-softening point oil products, but also suitable for determining low-content quinoline insoluble matter in coal tar and petroleum asphalt. Background Art

[0002] Quinoline insoluble matter is one of the important indicators of the quality of reaction materials. Especially in the carbon graphite manufacturing industry, in order to produce high-quality carbon graphite products, it is necessary to control the quinoline insoluble matter content in coal tar and ensure that the raw materials have low quinoline insoluble matter content, high coking value and high β resin.

[0003] The principle of determining quinoline insolubles is: a certain mass of sample is dissolved with quinoline under certain determination conditions, filtered, weighed to constant weight, and the mass of the insolubles is calculated as a percentage of the original sample mass. The current test methods include "GBT2293-2019 Test Method for Quinoline Insolubles in Coking Asphalt Products" and "Test Method for Determining Low-Content Quinoline Insolubles" developed by Tian Li et al. The above method is more convenient and accurate for analyzing samples with softening points ≤100°C and quinoline insolubles ≤10%. However, for special asphalts with softening points >100°C, such as coated asphalts with softening points of 250°C or even above 280°C, and quinoline insolubles >25%, the above method is used. In the actual analysis process, due to the sampling volume and temperature drop, some substances precipitate from quinoline to form aggregates and block the filter pores, resulting in the inability to continue filtration or the measured data being larger than the actual value. Summary of the invention

[0004] In view of the above-mentioned defects existing in the prior art, the purpose of the present invention is to provide a method for determining quinoline insoluble matter in a high softening point material, which can minimize the weighing error and avoid the phenomenon of inaccurate analysis results caused by clogging of filter holes due to temperature drop during the filtration process; the present invention has the advantages of short time consumption, fast results, high data accuracy and precision, good reproducibility and reproducibility, etc.

[0005] To achieve the above object, the present invention adopts the following technical solution:

[0006] The present invention provides a method for determining quinoline insoluble matter in a high softening point material, comprising the following steps:

[0007] S1, grind the high softening point material into powder, take 0.5-3g as a sample and put it in a beaker, pour 10-15ml quinoline into it, and heat it on an electric furnace to the sample dissolution temperature;

[0008] S2, after heating to the dissolution temperature of the sample, continue heating to increase the temperature by 30-80°C, stir for 2-5 minutes, and immediately transfer the feed liquid to a preheated sand star funnel for suction filtration to obtain a filter cake;

[0009] S3, using cold toluene to wash away the quinoline remaining on the filter cake, then drying the star funnel together with the filter cake, and then transferring them to a dryer for cooling and weighing and calculation.

[0010] Preferably, in step S1:

[0011] The particle size of the high softening point material powder is below 150 mesh; and / or

[0012] When the softening point of the high-softening-point material is less than 180°C, the mass of the sample is 1 to 3 g; when the softening point of the high-softening-point material is 180 to 230°C, the mass of the sample is 1 to 2 g; when the softening point of the high-softening-point material is greater than 230°C, the mass of the sample is 0.5 to 1.5 g; and / or

[0013] Preferably, in step S1:

[0014] The heating time is 10 to 30 minutes; and / or

[0015] The dissolution temperature of the sample is 20-30° C. higher than the softening point of the high-softening-point material.

[0016] Preferably, in step S1, the sample dissolution temperature is ≤340°C.

[0017] Preferably, in step S2, the preheating temperature of the star funnel is 150-200°C.

[0018] Preferably, in step S2, after the feed liquid is transferred to the preheated star funnel, 10 to 15 ml of hot quinoline is placed in the beaker, the residue on the beaker is thoroughly swept into the hot quinoline, and immediately poured into the star funnel for suction filtration, and then the above operation is repeated using 5 to 10 ml of hot quinoline.

[0019] Preferably, the temperature of the hot quinoline is equal to the sample dissolution temperature in step S1.

[0020] Preferably, in step S3, the filter cake is washed with cold toluene twice, and the amount of each wash is 20-40 ml.

[0021] Preferably, in step S3, during the drying process, the drying temperature is 150-200° C., and the drying time is 15-30 min.

[0022] Preferably, in step S3, the drying star funnel and the filter cake are taken out of the oven and naturally cooled for 2 to 3 minutes before being cooled again; and / or

[0023] The cooling time of the cooling treatment is 20 to 30 minutes.

[0024] The method for determining quinoline insoluble matter in a high softening point material provided by the present invention has the following beneficial effects:

[0025] 1. The present invention is suitable for detecting the content of quinoline insolubles in high softening point materials (>100°C), and is also suitable for detecting the content of quinoline insolubles in common samples (softening point ≤100°C); the present invention can reduce the weighing error to the maximum extent, and avoid the clogging of the filter holes due to the temperature drop during the filtration process, thereby causing the analysis failure or the filtration time to be extended by several times, and finally leading to the occurrence of inaccurate analysis results, time-consuming and labor-intensive phenomena, etc.;

[0026] 2. The present invention grinds the sample into powder according to its different softening points, takes different amounts, and greatly increases the quinoline temperature under the premise of ensuring safety and no chemical reaction, so that the quinoline soluble matter in the sample is fully dissolved in quinoline. At the same time, the filter is preheated to a relatively high temperature, and filtered while hot, ensuring that the entire filtration and washing time is within 10 to 15 minutes, so as to avoid the pores being blocked due to temperature drop, and the filtration cannot be continued, resulting in analysis failure;

[0027] 3. The present invention has the advantages of short time consumption, fast result, high data accuracy and precision, and good reproducibility and reproducibility. DETAILED DESCRIPTION

[0028] In order to better understand the above technical solution of the present invention, the technical solution of the present invention is further described below in conjunction with embodiments.

[0029] The existing analysis method is only applicable to samples with a softening point and a content of quinoline insolubles that is not too high. When analyzing samples with a softening point higher than 100°C, due to the temperature drop, some substances precipitate from quinoline to form aggregates and block the filter holes, requiring the filtration time to be extended by multiples, or even resulting in the situation where the filtration cannot be continued. Therefore, the present invention develops a method suitable for detecting high softening point materials (>100°C) and quinoline insolubles in ordinary samples. The present invention can minimize the weighing error, and at the same time avoid the blockage of the filter holes caused by the temperature drop during the filtration process, resulting in analysis failure or the filtration time being extended by multiples, which ultimately leads to inaccurate analysis results, no reference value, and time-consuming and labor-intensive.

[0030] A method for determining quinoline insoluble matter in a high softening point material of the present invention comprises the following steps:

[0031] S1, grind the high softening point material into powder, take 0.5-3g as a sample and put it in a beaker, pour 10-15ml quinoline into it, and heat it on an electric furnace to the sample dissolution temperature;

[0032] Specifically, the high softening point material is ground into powder with a particle size of less than 150 meshes by a pulverizer, 0.5-3g is taken as a sample and placed in a 50ml beaker, 10-15ml quinoline is poured in, and the beaker is placed in an electric furnace and heated for 10-30min to reach the sample dissolution temperature, which is preferably the actual temperature. The sampling amount of the sample is different for materials with different softening points. In a specific embodiment, when the softening point of the high softening point material is less than 180°C, the mass of the sample is 1-3g; when the softening point of the high softening point material is 180-230°C, the mass of the sample is 1-2g; when the softening point of the high softening point material is greater than 230°C, the mass of the sample is 0.5-1.5g. In a specific embodiment, the sample dissolution temperature is 20-30°C higher than the softening point of the high softening point material, that is, the sample dissolution temperature is the sample softening point + 20-30°C; the maximum value of the sample dissolution temperature is ≤235°C.

[0033] S2, after heating to the dissolution temperature of the sample, continue heating to increase the temperature by 30-80°C, stir for 2-5 minutes, and immediately transfer the liquid to a preheated sand star funnel for suction filtration to obtain a filter cake;

[0034] Specifically, after heating to the sample dissolution temperature, continue heating to increase the temperature by 30 to 80°C, stir for 2 to 5 minutes, take out the preheated star funnel placed in a 150 to 200°C oven, and immediately transfer the liquid in the beaker to the preheated star funnel for filtration. After the filtration, a filter cake is obtained. At the same time, in order to minimize the error, after transferring the liquid in the beaker to the star funnel, take 10 to 15 ml of hot quinoline and place it in the beaker. Use a glass rod to thoroughly clean the mouth, wall and bottom residue of the beaker into the hot quinoline, and immediately pour it into the star funnel for filtration, and then repeat the above operation with 5 to 10 ml of hot quinoline. In the above process, the preheating temperature of the star funnel is 150 to 200°C. The temperature of the hot quinoline used when cleaning the beaker is equal to the temperature of the liquid.

[0035] S3, use cold toluene to wash away the quinoline remaining on the filter cake, then dry the star funnel together with the filter cake, and then transfer it to a dryer for cooling and weighing and calculation.

[0036] Specifically, cold toluene is used to wash away the quinoline remaining on the filter cake, which can be washed twice, with an amount of 20 to 40 ml for each wash. After the completion, the star funnel and the filter cake are placed in an oven for drying, the drying temperature is 150 to 200° C., and the drying time is 15 to 30 minutes; the star funnel and the filter cake after the drying treatment are taken out of the oven and naturally cooled for 2 to 3 minutes, and then the dried star funnel and the filter cake are transferred to a dryer for cooling treatment and weighed and calculated; wherein the cooling time for the cooling treatment is 20 to 30 minutes.

[0037] The method for determining quinoline insoluble matter in high softening point materials of the present invention is further described below with reference to specific examples.

[0038] Example 1

[0039] A method for determining quinoline insoluble matter in a high softening point material in the present embodiment, the specific process is as follows:

[0040] Weigh 2.5g of medium-temperature asphalt (softening point 86°C) in a 50ml beaker, add 12ml of quinoline, place it on an electric furnace and heat it to 110°C. After the temperature is reached, continue to heat it to 180°C, stir it for 2-5min, and immediately transfer it to a sand star funnel preheated to 150°C for suction filtration. Take 15ml of 110°C hot quinoline and place it in a 50ml beaker. Use a glass rod to thoroughly sweep the cup mouth, wall and bottom residues into the hot quinoline, and immediately pour it into the funnel for suction filtration. Then take 10ml of hot quinoline and repeat the above steps once. After completion, a filter cake is obtained. Wash the quinoline in the filter cake with 20ml of cold toluene twice, and then put the funnel with the filter cake into a 150°C oven for drying for 20min. After the drying treatment, take the sand star funnel and the filter cake out of the oven and cool them naturally for 2-3min. Finally, transfer them to a dryer and cool them for 20min before weighing and calculating. The results are shown in the following table:

[0041]

[0042]

[0043] Example 2

[0044] A method for determining quinoline insoluble matter in a high softening point material in the present embodiment, the specific process is as follows:

[0045] Weigh 3g of soft asphalt (softening point 35℃) in a 50ml beaker, add 10ml of quinoline, place on an electric furnace and heat to 65℃. After the temperature is reached, continue to heat to 120℃, stir for 2-5min, and immediately transfer to a sand star funnel preheated to 150℃ for suction filtration. Take 10ml of 65℃ hot quinoline and place it in a 50ml beaker. Use a glass rod to thoroughly sweep the cup mouth, wall and bottom residues into the hot quinoline, and immediately pour it into the funnel for suction filtration. Then take 5ml of hot quinoline and repeat the above steps once. After completion, a filter cake is obtained. Wash the quinoline in the filter cake with 20ml of cold toluene twice, and then put the funnel with the filter cake into a 150℃ oven for drying for 15min. After the drying treatment, take the sand star funnel and the filter cake out of the oven and cool naturally for 2-3min. Finally, transfer it to a dryer and cool for 15min before weighing and calculating. The results are shown in the following table:

[0046]

[0047] Example 3

[0048] A method for determining quinoline insoluble matter in a high softening point material in the present embodiment, the specific process is as follows:

[0049] Weigh 1.5g of high softening point asphalt (softening point 205℃) in a 50ml beaker, add 15ml of quinoline, place on an electric furnace and heat to 225℃. After reaching the temperature, continue to heat to 300℃, stir for 2-5min, and immediately transfer to a sand star funnel preheated to 180℃ for suction filtration. Take 15ml of 225℃ hot quinoline and place it in a 50ml beaker. Use a glass rod to thoroughly sweep the cup mouth, wall and bottom residues into the hot quinoline, and immediately pour it into the funnel for suction filtration. Then take 10ml of hot quinoline and repeat the above steps once. After completion, a filter cake is obtained. Wash the quinoline in the filter cake with 30ml of cold toluene twice, and then put the funnel with the filter cake into a 160℃ oven for drying for 30min. After the drying treatment, take the sand star funnel and the filter cake out of the oven and cool naturally for 2-3min. Finally, transfer it to a dryer and cool for 30min before weighing and calculating. The results are shown in the following table:

[0050]

[0051] Example 4

[0052] A method for determining quinoline insoluble matter in a high softening point material in the present embodiment, the specific process is as follows:

[0053] Weigh 1g of high softening point asphalt (softening point 225℃) in a 50ml beaker, add 15ml of quinoline, place on an electric furnace and heat to 250℃. After reaching the temperature, continue to heat to 300℃, stir for 2-5min, and immediately transfer to a sand star funnel preheated to 160℃ for suction filtration. Take 15ml of 250℃ hot quinoline and place it in a 50ml beaker. Use a glass rod to thoroughly sweep the cup mouth, wall and bottom residues into the hot quinoline, and immediately pour it into the funnel for suction filtration. Then take 10ml of hot quinoline and repeat the above steps once. After completion, a filter cake is obtained. Wash the quinoline in the filter cake with 30ml of cold toluene twice, and then put the funnel with the filter cake into a 190℃ oven for drying for 15min. After the drying treatment, take the sand star funnel and the filter cake out of the oven and cool naturally for 2-3min. Finally, transfer it to a dryer and cool for 15min before weighing and calculating. The results are shown in the following table:

[0054]

[0055] Example 5

[0056] A method for determining quinoline insoluble matter in a high softening point material in the present embodiment, the specific process is as follows:

[0057] Weigh 0.5g of high softening point asphalt (softening point 282℃) in a 50ml beaker, add 15ml quinoline, place on an electric furnace and heat to 305℃. After reaching the temperature, continue to heat to 340℃, stir for 2-5min, and immediately transfer to a sand star funnel preheated to 200℃ for suction filtration. Take 15ml of 235℃ hot quinoline and place it in a 50ml beaker. Use a glass rod to thoroughly clean the cup mouth, wall and bottom residues into the hot quinoline, and immediately pour it into the funnel for suction filtration. Then take 10ml of hot quinoline and repeat the above steps once. After completion, a filter cake is obtained. Wash the quinoline in the filter cake with 40ml cold toluene twice, and then put the funnel with the filter cake into a 200℃ oven for drying for 25min. After the drying treatment, take the sand star funnel and the filter cake out of the oven and cool naturally for 2-3min. Finally, transfer it to a dryer and cool for 25min before weighing and calculating. The results are shown in the following table:

[0058]

[0059] Those skilled in the art should recognize that the above embodiments are only used to illustrate the present invention, and are not intended to limit the present invention. As long as they are within the spirit of the present invention, any changes or modifications to the above embodiments will fall within the scope of the claims of the present invention.

Claims

1. A method for determining quinoline insoluble matter in a high softening point material, characterized in that: The following steps are involved: S1, grind the high softening point material into powder, take 0.5-3g as a sample and put it in a beaker, pour 10-15ml quinoline into it, and heat it on an electric furnace to the sample dissolution temperature; S2, after heating to the dissolution temperature of the sample, continue heating to increase the temperature by 30-80°C, stir for 2-5 minutes, and immediately transfer the liquid in the beaker to a preheated star funnel for suction filtration to obtain a filter cake; S3, using cold toluene to wash away the quinoline remaining on the filter cake, then drying the star funnel together with the filter cake, and then transferring them to a dryer for cooling and weighing and calculation.

2. The method for measuring quinoline insolubles in high softening point materials according to claim 1, characterized in that: In step S1: The particle size of the high softening point material powder is below 150 mesh; and / or When the softening point of the high-softening-point material is less than 180°C, the mass of the sample is 1 to 3g; when the softening point of the high-softening-point material is 180 to 230°C, the mass of the sample is 1 to 2g; when the softening point of the high-softening-point material is greater than 230°C, the mass of the sample is 0.5 to 1.5g.

3. The method for measuring quinoline insolubles in high softening point materials according to claim 1, characterized in that: In step S1: The heating time is 10 to 30 minutes; and / or The dissolution temperature of the sample is 20-30° C. higher than the softening point of the high-softening-point material.

4. The method for measuring quinoline insolubles in high softening point materials according to claim 3, characterized in that: In the step S1, the sample dissolution temperature is ≤340°C.

5. The method for measuring quinoline insoluble matter in high softening point materials according to claim 1, characterized in that: In step S2, the preheating temperature of the star funnel is 150-200°C.

6. The method for measuring quinoline insoluble matter in high softening point materials according to claim 1, characterized in that: In step S2, after the feed liquid is transferred to the preheated star funnel, 10 to 15 ml of hot quinoline is placed in the beaker, the residue on the beaker is thoroughly swept into the hot quinoline, and immediately poured into the star funnel for suction filtration, and then the above operation is repeated using 5 to 10 ml of hot quinoline.

7. The method for measuring quinoline insoluble matter in high softening point materials according to claim 6, characterized in that: The temperature of the hot quinoline is equal to the sample dissolution temperature in step S1.

8. The method for measuring quinoline insoluble matter in high softening point materials according to claim 1, characterized in that: In the step S3, the filter cake is washed with the cold toluene twice, and the amount used for each washing is 20-40 ml.

9. The method for measuring quinoline insoluble matter in high softening point materials according to claim 1, characterized in that: In the step S3, during the drying process, the drying temperature is 150-200° C. and the drying time is 15-30 minutes.

10. The method for determining quinoline insoluble matter in a high softening point material according to claim 1, characterized in that: In step S3: After the drying treatment, the star funnel and the filter cake are taken out of the oven and naturally cooled for 2 to 3 minutes, and then subjected to cooling treatment; and / or The cooling time of the cooling treatment is 20 to 30 minutes.

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