Method for rapidly measuring coking value of oil product

Abstract

The invention discloses a method for rapidly measuring the coking value of an oil product. The method comprises the following steps: S1, sampling preparation; s2, finely taking a sample, and placing the sample in a crucible; s3, placing the crucible in an ark; s4, the ark is placed in a tubular furnace, and nitrogen is used for replacing air; s5, the tubular furnace is heated; and S6, after keeping the temperature constant, increasing the nitrogen amount, cooling to room temperature, taking out the sample from the tubular furnace, weighing, and calculating a result. According to the coking value principle processing, the coking value measuring method which is short in testing time, fast in data result obtaining, high in accuracy and precision, good in reproducibility and small in human and external interference factors is provided.

Description

Technical Field

[0001] The invention relates to a method for quickly determining the coking value of oil products. Background Art

[0002] The coking value is the amount of coke formed when oil products are partially burned at high temperatures. It is a key indicator for measuring oil product characteristics and final product quality. At present, the only method for determining the coking value is the national standard method "Determination of the coking value of coal tar products" GB / T8727-2008, or an improved enterprise standard based on this national standard method. However, no matter which method is used, the test time is relatively long (generally about 2.5 to 3 hours to get the result), and the selection of symmetrical sample quantity and filler is more restrictive, and the operation flexibility is small. For quality monitoring indicators of mature and stable processes, the national standard is feasible. However, for research and development, it is urgent to adjust the subsequent processes according to the coking value, and the national standard is not very applicable, and the test time will seriously hinder the progress of the project. Therefore, there is an urgent need for a determination method that is fast and simple, with few interference factors, accurate results, and high credibility. Summary of the invention

[0003] In view of the defects of the prior art Chinese standard method for coking value, which has a long time to produce data and low operational flexibility, the purpose of the present invention is to provide a method for quickly determining the coking value of oil products. Based on the principle of coking value, a method for determining the coking value is proposed, which has the advantages of short testing time, fast data production, high accuracy and precision, good reproducibility, and little influence by human and external interference factors.

[0004] To achieve the above object, the present invention adopts the following technical solution:

[0005] A method for quickly determining the coking value of oil products comprises the following steps:

[0006] S1. Sampling preparation;

[0007] S2, carefully take the sample and place it in a crucible;

[0008] S3. Place the crucible in the ark;

[0009] S4. Place the ark in a tube furnace and replace the air with nitrogen;

[0010] S5, heating up the tube furnace;

[0011] S6. After maintaining constant temperature, increase the amount of nitrogen to cool down to room temperature, take out the sample from the tube furnace, weigh it, and calculate the result.

[0012] Preferably, in step S1, the sample is a solid sample or a liquid sample;

[0013] If the sample is solid, the sampling amount is 50g, and then a grinder is used to grind the sample into powder for 30 to 60 seconds.

[0014] Preferably, the particle size of the powdered sample is ≤80 mesh.

[0015] Preferably, in step S2, if the sample is solid, 0.5 to 5 g of the sample is accurately taken;

[0016] If the sample is liquid, take 1 to 3 mL of the sample accurately;

[0017] And then placed in a 20mL ceramic crucible with a lid that has been weighed constant.

[0018] Preferably, in step S4, the air is replaced with nitrogen for 10 to 15 minutes.

[0019] Preferably, in step S5, the nitrogen flow rate is adjusted to 20-30 mL / min, the tubular furnace starts heating, and the temperature is raised to 550±10° C. within 10-15 minutes.

[0020] Preferably, in step S6, the constant temperature time is 15 to 30 minutes;

[0021] Increase the nitrogen flow rate to 150-350 ml / min.

[0022] Preferably, the coking value is calculated as follows:

[0023] Coking value = [(m (坩埚+样品) -m 坩埚 ) / m 样品 】*100%;

[0024] In the formula, m (坩埚+样品) It indicates the gross weight of the sample after heat treatment at 550±10℃ for 2h, in g;

[0025] m 坩埚 Indicates the mass of the crucible, in g;

[0026] m 样品 It indicates the mass of the sample before heat treatment, in g.

[0027] The method for quickly determining the coking value of oil products provided by the present invention can shorten the time for obtaining test data to 60 to 120 minutes, and nitrogen is used to replace air, completely eliminating oxygen, and ensuring the authenticity of the results. Heating and cooling are all under nitrogen protection, avoiding the introduction of air during the process of taking out the sample and putting it into the dryer to cool to room temperature, which causes the final result to be higher than the true value. At the same time, when sampling, both the tubular furnace and the sample are at room temperature, avoiding the risk of scalding when the national standard uses a muffle furnace and the door is opened for sampling. 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 present invention provides a method for quickly determining the coking value of oil products, comprising the following steps:

[0030] S1. Sampling preparation;

[0031] The sample is a solid sample or a liquid sample;

[0032] If the sample is solid, the sample size is 50 g, and then the sample is crushed into powder using a grinder for 30 to 60 seconds;

[0033] The particle size of powdered samples is ≤80 mesh.

[0034] S2. Take the sample carefully and place it in a 20 mL ceramic crucible with a lid that has been weighed constant;

[0035] If the sample is solid, take 0.5 to 5 g of sample accurately;

[0036] If the sample is liquid, accurately take 1 to 3 mL of the sample.

[0037] S3. Place the crucible stably in the ark.

[0038] S4. Place the ark in a tube furnace and replace the air with nitrogen for 10 to 15 minutes.

[0039] S5. Adjust the nitrogen flow rate to 20-30 mL / min, start heating in the tubular furnace, and raise the temperature to 550±10°C within 10-15 minutes.

[0040] S6. Keep the temperature at 550±10℃ for 15-30min, increase the nitrogen flow rate to 150-350ml / min, and then quickly cool to room temperature. Take out the sample from the tube furnace, weigh it, and calculate the result.

[0041] The coking value is calculated as follows:

[0042] Coking value = [(m (坩埚+样品) -m 坩埚 ) / m 样品 】*100%;

[0043] In the formula, m (坩埚+样品) It means the gross weight of the sample after heat treatment at 550±10℃ for 2h, in g;

[0044] m 坩埚 Indicates the mass of the crucible, in g;

[0045] m 样品 Indicates the mass of the sample before heat treatment, in g.

[0046] Example 1

[0047] In this Example 1, 3.1234 g, 2.1594 g, 1.2326 g and 2.1563 g of coal tar soft pitch were weighed in sequence and placed in 20 mL covered porcelain crucibles, recorded as 1#, 2#, 3# and 4#, placed in an ark, placed in a tubular furnace, and nitrogen replaced for 10 minutes. The temperature was raised to 550° C. within 10 minutes, with a nitrogen flow rate of 20 mL / min. After the temperature was kept constant for 30 minutes, the nitrogen flow rate was adjusted to 200 mL / min. After cooling to room temperature, the crucible was taken out and weighed and calculated, as follows:

[0048]

[0049] Example 2

[0050] In this Example 2, 1.3234 g, 1.1594 g, 2.2326 g and 3.1563 g of 110°C modified asphalt were weighed in turn and placed in 20 mL covered porcelain crucibles, recorded as 1#, 2#, 3# and 4#, placed in an ark, placed in a tubular furnace, and nitrogen replaced for 12 minutes, and then heated to 550°C within 15 minutes, with a nitrogen flow rate of 25 mL / min. After constant temperature for 15 minutes, the nitrogen flow rate was adjusted to 350 mL / min, and the crucible was taken out after cooling to room temperature and weighed and calculated, as follows:

[0051]

[0052] Example 3

[0053] Example 3 3.0234 g, 1.1214 g, 3.1326 g and 2.1763 g of 250°C special asphalt were weighed in turn and placed in 20 mL covered porcelain crucibles, recorded as 1#, 2#, 3# and 4#, placed in an ark, placed in a tubular furnace, and nitrogen replaced for 15 minutes. The temperature was raised to 550°C within 13 minutes, with a nitrogen flow rate of 30 mL / min. After constant temperature for 20 minutes, the nitrogen volume was adjusted to 150 mL / min. After cooling to room temperature, the crucible was taken out and weighed and calculated, as follows:

[0054]

[0055] Example 4

[0056] Example 4 1.4341 g, 2.6214 g, 1.1306 g and 3.1963 g of 106°C coumarone were weighed in sequence and placed in 20 mL covered porcelain crucibles, recorded as 1#, 2#, 3# and 4#, placed in an ark, placed in a tubular furnace, and nitrogen replaced for 10 min. The temperature was raised to 550°C within 15 min, with a nitrogen flow rate of 20 mL / min. After constant temperature for 25 min, the nitrogen flow rate was adjusted to 300 mL / min. After cooling to room temperature, the crucible was taken out and weighed and calculated, as follows:

[0057]

[0058] Example 5

[0059] Example 5 2.1341 g, 2.9214 g, 2.6306 g and 2.1363 g of ethylene tar were weighed in turn and put into 20 mL covered porcelain crucibles, recorded as 1#, 2#, 3# and 4#, put into an ark, placed in a tube furnace, and nitrogen replaced for 15 minutes. The temperature was raised to 550°C within 15 minutes, with a nitrogen flow rate of 30 mL / min. After keeping the temperature constant for 30 minutes, the nitrogen flow was adjusted to 180 mL / min. After cooling to room temperature, the crucible was taken out and weighed and calculated, as follows:

[0060]

[0061] Example 6

[0062] Example 6 Weigh 0.8550g, 0.8546g, 0.8572g and 0.8561g of washing oil (liquid at room temperature) in turn and put them into 20mL covered porcelain crucibles, record them as 1#, 2#, 3# and 4#, put them into an ark, place them in a tube furnace, replace with nitrogen for 10 minutes, heat to 550°C within 10 minutes, nitrogen flow rate is 30mL / min, keep constant temperature for 20 minutes, adjust nitrogen flow rate to 220mL / min, cool to room temperature, take out the crucible and weigh and calculate, as follows:

[0063]

[0064]

[0065] 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 quickly determining the coking value of oil products, It is characterized in that The following steps are involved: S1. Sampling preparation; S2, carefully take the sample and place it in a crucible; S3. Place the crucible in the ark; S4. Place the ark in a tube furnace and replace the air with nitrogen; S5, heating up the tube furnace; S6. After maintaining constant temperature, increase the amount of nitrogen to cool down to room temperature, take out the sample from the tube furnace, weigh it, and calculate the result.

2. The method for rapidly determining the coking value of oil products according to claim 1, Features: In step S1, the sample is a solid sample or a liquid sample; If the sample is solid, the sampling amount is 50g, and then a grinder is used to grind the sample into powder for 30 to 60 seconds.

3. The method for rapidly determining the coking value of oil products according to claim 2, Features: The particle size of powdered samples is ≤80 mesh.

4. The method for rapidly determining the coking value of oil products according to claim 2, Features: In step S2, if the sample is solid, accurately take 0.5 to 5 g of the sample; If the sample is liquid, take 1 to 3 mL of the sample accurately; And then placed in a 20mL ceramic crucible with a lid that has been weighed constant.

5. The method for rapidly determining the coking value of oil products according to claim 4, Features: In step S4, the air is replaced with nitrogen for 10 to 15 minutes.

6. The method for rapidly determining the coking value of oil products according to claim 5, Features: In step S5, the nitrogen flow rate is adjusted to 20-30 mL / min, the tubular furnace starts heating, and the temperature is raised to 550±10° C. within 10-15 minutes.

7. The method for rapidly determining the coking value of oil products according to claim 6, Features: In step S6, the constant temperature time is 15 to 30 minutes; Increase the nitrogen flow rate to 150-350 ml / min.

8. The method for rapidly determining the coking value of oil products according to claim 6, It is characterized in that The coking value is calculated as follows: Coking value = [(m (坩埚+样品) -m 坩埚 ) / m 样品 】*100%; In the formula, m (坩埚+样品) It means the gross weight of the sample after heat treatment at 550±10℃ for 2h, in g; m 坩埚 Indicates the mass of the crucible, in g; m 样品 It indicates the mass of the sample before heat treatment, in g.

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