CN111595795B - Method for evaluating storage stability of heavy modified oil - Google Patents
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- 230000032683 aging Effects 0.000 claims abstract description 65
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- 238000002371 ultraviolet--visible spectrum Methods 0.000 claims abstract description 11
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Abstract
The invention belongs to the field of heavy modified oil modification processing, and particularly relates to a novel method for evaluating the storage stability of heavy modified oil. The method comprises the following specific steps: placing heavy modified oil into a reaction kettle, aging for a certain time (5-24 h) at a certain aging temperature (80-120 ℃) by taking air as an aging atmosphere, taking out the modified oil, dissolving the modified oil into a certain volume of solvent for ultraviolet-visible spectrum measurement, scanning the absorbance change of an oil sample in the wavelength range of 400-800 nm, integrating the absorbance in the range with the wavelength of a visible light region, and defining delta S when the aging time is 0h A Is 0, the change value deltaS of the integral area is obtained A The long-term storage stability of the oil product is quantitatively evaluated by taking the long-term storage stability as an index. The method has important significance for quickly evaluating the long-term storage stability of the heavy modified oil.
Description
Technical Field
The invention belongs to the field of heavy modified oil modification processing, and particularly relates to a novel method for evaluating the stability of heavy modified oil.
Background
The global demand for petroleum resources is continuously increased, the exploitation output of the conventional petroleum resources in the world is limited, and in order to meet the increasing demand for crude oil in the world, people pay attention to the development of heavy unconventional petroleum resources. These unconventional petroleum resources, which are characterized by high viscosity, low API level, high content of heteroatoms and asphaltenes, encounter a number of difficulties in transportation, marketing and subsequent processing. The heavy oil thermal processing has the advantages of mature technology, low investment cost and the like, and is one of important heavy oil upgrading and processing means. At present, corresponding heavy oil upgrading plants are established in some countries and regions in the world, most of the upgrading plants take delayed coking or fluid coking as core devices, and the processes are thermal processing processes. However, the stability of the modified oil obtained by the thermal processing process is low. During storage and transportation, the phase separation phenomenon is easily generated, insoluble sediments such as asphaltene are generated, and great harm is brought to storage and transportation of oil products. During long-distance transportation, the phase separation is shown to increase the viscosity of oil products, thereby causing the energy consumption of oil transportation to increase; on the other hand, the generated asphaltene insoluble substances may deposit on pipelines and oil transportation equipment, affecting the oil transportation efficiency, even causing pipeline blockage or causing the equipment to work abnormally. In the process of long-term storage in a ship or a storage tank, generated insoluble substances can be deposited and deposited at the bottom of the tank to form semi-solid sediment, so that the ship is difficult to unload, potential safety hazards are generated in the storage process, and the storage process is challenged. During the refining process, the phase separation of the asphaltenes can cause coking of pipelines and equipment, blockage of the pipelines and damage to the equipment; the heat exchanger is scaled, so that the heat exchange efficiency is reduced; adsorption to the catalyst surface, causing catalyst deactivation, and the like. In order to ensure the proper operation of the above process, the poor quality heavy upgraded oil must be evaluated for long term storage stability prior to its transportation and storage. The conventional evaluation method for the stability of the oil product mainly determines the deposition starting point of the asphaltene according to the difficulty of phase separation of the asphaltene in a petroleum system, and comprises a viscosity method, a conductivity method, an optical method, an interfacial tension method, a drop diffusion method, a calorimetry method and a spot test method. However, the above method is mainly suitable for evaluating the short-term stability of oil products but not suitable for evaluating the long-term storage stability of oil products.
CN102288744B discloses a method for determining oil product stability according to sample property changes at different storage times by using a 10-50 m tubular column to simulate storage and transportation conditions of heavy oil transported by an oil tanker, however, the method is not suitable for evaluating the storage stability of modified oil simply and quickly in a laboratory.
Zhang Na et al (journal of fuel chemistry, 38 (6), 2010; chemical engineering progress, 34 (8), 2015) and CN104764678a disclose methods for evaluating long-term storage stability of venezuela orii slag viscosity-reduced products, viscosity-reduced blend oils and other fuel oils, all of which use detailed property changes of stock oils after storage for different days (different from 20 to 90 days) under different conditions as determination indicators, and have disadvantages of long test time and complicated test process.
Therefore, it is necessary to establish a method for rapidly and accurately evaluating the long-term storage stability of the heavy modified oil, which provides an important basis for predicting the phase separation behavior of the heavy modified oil during long-distance transportation and storage.
Disclosure of Invention
The invention relates to a novel method for evaluating the stability of heavy modified oil, which can simply, conveniently, quickly and accurately evaluate the long-term storage stability of the heavy modified oil and has important practical guiding significance for predicting the phase separation behavior of inferior heavy modified oil in the processes of long-distance transportation and long-term storage.
In order to achieve the purpose, the invention provides the following technical method:
the invention provides a method for evaluating the storage stability of heavy modified oil, which comprises the following steps:
(1) Placing heavy modified oil in a reaction kettle, taking air or oxygen as an aging atmosphere, heating to an aging temperature, and taking out the aged modified oil;
(2) Dissolving the aged modified oil sample in a solvent, performing ultraviolet-visible spectrum measurement, and scanning to obtain the absorbance of the oil sample in the wavelength range of 400-800 nm;
(3) Integrating the absorbance on the wavelength of the visible light region, and defining delta S when the aging time is 0h A Is 0, the change value deltaS of the integral area is obtained A 。
The invention provides a method for evaluating the storage stability of heavy modified oil, wherein in the step (1), heating and temperature rise are carried out by adopting oil bath heating.
The invention provides a method for evaluating the storage stability of heavy modified oil, wherein the aging temperature in the step (1) is 80-120 ℃.
The invention provides a method for evaluating the storage stability of heavy modified oil, wherein in the step (1), the aging time is 5-24 h.
The invention provides a method for evaluating the storage stability of heavy modified oil, wherein the integration in the step (3) is carried out according to the following formula:
A＝f(λ)；
wherein A is the absorbance of the oil sample in the wavelength range of 400-800 nm; λ is the wavelength; and S is the integral area.
The invention provides a method for evaluating storage stability of heavy modified oil, wherein the heavy modified oil is an oil product obtained after heavy oil is subjected to a modification process.
The invention provides a method for evaluating storage stability of heavy modified oil, wherein the heavy modified oil is an oil product doped with diluent, visbreaking, hydrogen supply cracking or solvent deasphalting.
The invention provides a method for evaluating the storage stability of heavy modified oil, wherein the solvent is normal alkane or an aromatic hydrocarbon-normal alkane mixed solvent.
The invention provides a method for evaluating the storage stability of heavy modified oil, wherein the normal alkane is normal heptane.
The present invention can be described in detail as follows:
the invention provides a method for rapidly evaluating long-term storage stability of heavy modified oil, which is characterized by comprising the following steps of:
(1) Placing the heavy modified oil in a reaction kettle, heating to an aging temperature by taking air or oxygen as an aging atmosphere, and taking out the aged modified oil after a certain time;
(2) Dissolving the aged modified oil sample in a solvent, performing ultraviolet-visible spectrum measurement, and scanning to obtain the absorbance of the oil sample in the wavelength range of 400-800 nm;
(3) The absorbance in this range was integrated with the wavelength in the visible region, and Δ S at an aging time of 0h was defined A Is 0, the change value deltaS of the integral area is obtained A 。
Preferably, the aging temperature is 80-120 ℃;
preferably, the aging time is 5-24 h;
preferably, the integration is performed according to the following formula:
A＝f(λ)；
wherein A is the absorbance of the oil sample in the wavelength range of 400-800 nm; λ is the wavelength; s is the integral area;
preferably, the heavy upgraded oil is an oil product obtained after heavy oil is subjected to an upgrading process; more preferably diluted, visbroken, hydrogen-donating cracked, solvent deasphalted and other oil products.
Preferably, the solvent is a normal alkane or an aromatic hydrocarbon-normal alkane mixed solvent.
Preferably, the n-alkane is n-heptane.
Preferably, the mass ratio of the heavy upgraded oil to the solvent is determined according to the type of the solvent and the content of insoluble matters in the upgraded oil.
In more detail, the present invention can be operated as follows:
(1) Weighing 300g of heavy modified oil sample, placing the heavy modified oil sample in a reaction kettle, screwing the reaction kettle tightly, and carrying out an aging process by adopting the reaction kettle shown in figure 1;
(2) Taking air as an aging atmosphere, heating to a certain aging temperature (80-120 ℃), and taking out the aged modified oil after a certain time (5-24 h);
(3) Dissolving the aged modified oil sample in a solvent to prepare an oil sample-n-heptane solution with the concentration of about 1g/L, performing ultraviolet-visible spectrum measurement, and scanning to obtain the absorbance of the oil sample in the wavelength range of 400-800 nm;
(4) Defining the delta S when the aging time is 0h A Is 0, the absorbance in this range is integrated with the wavelength of the visible light region, and the change value Δ S of the integrated area is compared A The oil stability was evaluated and the integral was calculated according to the following formula: a = f (λ);
wherein A is the absorbance of the oil sample in the wavelength range of 400-800 nm; λ is the wavelength; and S is the integral area.
In summary, the invention takes heavy modified oil as raw material, aging test is carried out in a reaction kettle under certain aging temperature, aging time and air atmosphere, the aged modified oil is characterized by ultraviolet visible spectrum, the specific absorbance of the ultraviolet visible spectrum within 400-800 nm is integrated with the wavelength of the visible region, and the change value delta S of the integral area is used A As a quantitative index for evaluating the long-term storage stability of the upgraded oil.
The invention has the beneficial effects that:
the method for long-term storage stability of the heavy modified oil has the characteristics of short evaluation time and simple and convenient evaluation process, and the obtained result can provide an important basis for predicting the phase separation behavior of the heavy modified oil in the processes of long distance, long-term transportation and long storage.
Drawings
FIG. 1 shows a reaction vessel used in the examples, which is heated by an oil bath and equipped with a pressure gauge for monitoring the pressure in the vessel; placing heavy modified oil in a kettle, screwing the reaction kettle tightly, taking air as an aging atmosphere, heating in an oil bath to an aging temperature, and taking out the aged modified oil after a certain time; dissolving the aged modified oil in a solvent, performing ultraviolet-visible spectrum measurement, and scanning to obtain the absorbance of the oil sample in the wavelength range of 400-800 nm; the absorbance in this range was integrated with the wavelength in the visible region, and Δ S at an aging time of 0h was defined A Is 0, the change value deltaS of the integral area is obtained A 。
FIG. 2 is Δ S of the aging process of example 1DCA at 80 ℃ and 120 ℃ A Change over aging time.
FIG. 3 is Δ S of the aging process of example 2DCB at 80 ℃ and 120 ℃ A Change over aging time.
FIG. 4 shows example Δ S A Value versus comparative example n-heptane insoluble concentration.
Detailed Description
The following examples illustrate the invention in detail: the present example is carried out on the premise of the technical scheme of the present invention, and detailed embodiments and processes are given, but the scope of the present invention is not limited to the following examples, and the experimental methods without specific conditions noted in the following examples are generally performed according to conventional conditions.
Heating temperature rising mode
In the present invention, the heating method in the step (1) is not particularly limited, and oil bath heating is generally adopted because of the advantages of relatively high temperature, high heating rate and uniform heating.
Aging temperature
In the present invention, the aging temperature in step (1) is not particularly limited, but is usually in the range of 80 to 120 ℃, and if the aging temperature is lower than 80 ℃, the temperature is too low, and if the actual storage condition of the oil product is simulated, a long aging time is required, and the purpose of quickly and easily determining the storage stability cannot be achieved. If the aging temperature is higher than 120 ℃, the temperature is too high, and the reaction path of oil products which are oxidized and deteriorated to generate insoluble substances is changed, so that the aging and deterioration conditions under the actual storage conditions are greatly deviated.
Aging time
In the present invention, the aging time in the step (1) is not particularly limited, but is usually in the range of 5 to 24 hours, and if the aging time is less than 5 hours, the aging time is too short, and if the aging time reaches the state of actual storage of the simulated oil product, the aging temperature needs to be raised, but if the temperature is too high, the aging time deviates from the actual storage condition. If the aging time is longer than 24h, a great deal of time is consumed for evaluating the storage stability of the oil product, and the aim of quick and simple evaluation cannot be fulfilled.
Application object
The method for evaluating the storage stability of the heavy modified oil provided by the invention is mainly applied to the heavy modified oil, in particular to oil products blended with dilute oil, visbreaking oil, hydrogen supply oil or solvent deasphalting oil. Because the oil products contain a large amount of S, N, O heteroatom compounds, colloid, asphaltene and other unstable and easily-degenerated components, the method accelerates the degeneration of the modified oil by strengthening the storage condition of the modified oil, and realizes the quick and simple evaluation of the stability of the modified oil by adopting an ultraviolet-visible spectrum characterization means.
Selection of solvents
In the present invention, the organic solvent is not particularly limited, and an n-alkane or an aromatic hydrocarbon-n-alkane mixed solvent is generally used, and n-alkane is most preferably n-heptane, because the solvent has the advantages of being generally used in laboratories, low in toxicity, environmentally friendly, and easily available.
(1) Weighing 300g of heavy modified oil sample, placing the heavy modified oil sample in a reaction kettle, screwing the reaction kettle tightly, and carrying out an aging process by adopting the reaction kettle shown in figure 1;
(2) Taking air as an aging atmosphere, heating to a certain aging temperature (80-120 ℃), and taking out the aged modified oil after a certain time (5-24 h);
the aging process was carried out using the reaction kettle described in figure 1. The specific implementation method comprises the following steps:
(1) Weighing 300g of heavy modified oil sample, placing the heavy modified oil sample in a reaction kettle, and screwing the reaction kettle tightly;
(2) Taking air as an aging atmosphere, heating to a certain aging temperature (80-120 ℃), and taking out the aged modified oil after a certain time (5-24 h);
(3) Dissolving the aged modified oil sample in n-heptane to prepare an oil sample-n-heptane solution with the concentration of about 1g/L, performing ultraviolet and visible spectrum measurement, and scanning to obtain the absorbance of the oil sample in the wavelength range of 400-800 nm;
(4) Defining delta S when the aging time is 0h A Is 0, the absorbance in this range is integrated with the wavelength of the visible light region, and the change value Δ S of the integrated area is compared A The oil stability is evaluated, and the integral is calculated according to the following formula: a = f (λ);
wherein A is the absorbance of the oil sample in the wavelength range of 400-800 nm; λ is the wavelength; and S is the integral area.
Example 1
The method comprises the steps of weighing 300g of a sample by taking coking thermal modified oil A (DCA, the relative molecular mass of the DCA is about 308, the distillation range distribution is 350-420 ℃, the aromatic content is 28.89%, the colloid content is 9.56%, and the S, N content is 0.43% and 0.26% respectively) as raw materials, placing the sample in a reaction kettle shown in figure 1, screwing the reaction kettle tightly, carrying out aging tests of 5h,12h, 111h and 24h respectively at 80 ℃ (293.15K) and 120 ℃ (353.15K) in an air atmosphere, dissolving the aged modified oil in n-heptane to prepare a solution of 1g/L, carrying out ultraviolet-visible spectrum measurement, scanning the absorbance change of an oil sample in the wavelength range of 400 nm-800 nm, and integrating the absorbance in the range with the wavelength of a visible light region. Defining the delta S when the aging time is 0h A Is 0, the change value deltaS of the integral area of each sample is obtained A . Delta S of aged oil A The change with aging time is shown in fig. 2.
Example 2
The method comprises the steps of weighing 300g of a sample by taking coking thermal modified oil B (DCB, the relative molecular mass of the DCB is about 352, the distillation range distribution is 420-500 ℃, the aromatic content is 34.98%, the colloid content is 12.47%, the asphaltene content is 0.20%, and the S, N content is 0.50% and 0.32% respectively) as raw materials, placing the sample in a reaction kettle shown in figure 1, screwing the reaction kettle tightly, carrying out aging tests of 5h,12h, 11lh and 24h respectively at 80 ℃ (293.15K) and 120 ℃ (353.15K) in an air atmosphere, dissolving the aged modified oil in n-heptane to prepare a solution of 1g/L, carrying out ultraviolet visible spectrum measurement, scanning the absorbance change of the oil sample in the wavelength range of 400 nm-800 nm, and integrating the absorbance of the range on the wavelength of a visible light region. Defining the delta S when the aging time is 0h A Is 0, the change value deltaS of the integral area of each sample is obtained A . Delta S of aged oil A The change with aging time is shown in fig. 3.
Comparative example 1
As a measure of Δ S A As an evaluation of the long-term storage stability of the modified oil, the modified oils obtained in examples 1 and 2 at different aging times were measured for the content of insoluble substances in n-heptane, and the value of Δ S was measured A The values correlate with the n-heptane insoluble content and the results are shown in FIG. 4.
The two examples show the Δ S of the samples at the same temperature A The values showed a linear increasing trend with increasing aging time and the stability became worse. Delta S of samples obtained at higher ageing temperatures for the same ageing time A The larger the value, the worse the stability. As is evident from FIG. 4, during aging, Δ S A The value has a certain linear relation with the content of the n-heptane insoluble substances, so that the value can be used as a quantitative index for evaluating the long-term storage stability of the oil product. The method for long-term storage stability of the heavy modified oil has the characteristics of short evaluation time and simple and convenient evaluation process, and the obtained result can provide an important basis for predicting the phase separation behavior of the heavy modified oil in the processes of long distance, long-term transportation and long storage.
Claims (9)
1. A method for evaluating the storage stability of heavy upgraded oil, comprising the steps of:
(1) Placing heavy modified oil in a reaction kettle, taking air or oxygen as an aging atmosphere, heating to an aging temperature, and taking out the aged modified oil;
(2) Dissolving the aged modified oil sample in a solvent, performing ultraviolet-visible spectrum measurement, and scanning to obtain the absorbance of the oil sample in the wavelength range of 400-800 nm;
(3) Integrating the absorbance on the wavelength of the visible light region, and defining delta S when the aging time is 0h A Is 0, the variation value Delta S of the integral area is obtained A 。
2. The method for evaluating the storage stability of heavy upgraded oil according to claim 1, wherein the heating in step (1) is carried out by oil bath heating.
3. The method for evaluating the storage stability of heavy upgraded oil according to claim 1, wherein the aging temperature in step (1) is 80-120 ℃.
4. The method for evaluating the storage stability of heavy upgraded oil according to claim 1, wherein the aging time in step (1) is 5 to 24 hours.
5. The method for evaluating the storage stability of a heavy upgraded oil according to claim 1, wherein the integration in the step (3) is performed according to the following formula:
A＝f(λ)；
wherein A is the absorbance of the oil sample in the wavelength range of 400-800 nm; λ is the wavelength; and S is the integral area.
6. The method for evaluating the storage stability of a heavy upgraded oil according to claim 1, wherein the heavy upgraded oil is an oil product obtained after heavy oil is subjected to an upgrading process.
7. The method of evaluating the storage stability of a heavy upgraded oil of claim 1, wherein the heavy upgraded oil is an oil that is blended with a diluent, visbroken, hydrogen donor cracked, or solvent deasphalted.
8. The method of evaluating the storage stability of a heavy upgraded oil of claim 1, wherein the solvent is a normal alkane or an aromatic hydrocarbon-normal alkane mixed solvent.
9. The method of evaluating the storage stability of a heavy upgraded oil of claim 8, wherein the n-alkane is n-heptane.
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