CN114280216A - A kind of method for measuring oil content of oil sand - Google Patents

Abstract

The invention provides a method for measuring oil content of oil sand. The method comprises the following steps: carrying out a combustion test by using oil sand standard samples with different known oil contents to obtain the total amount of carbon monoxide and carbon dioxide generated by the combustion of the oil sand standard samples with different oil contents, and further obtaining a crude oil combustion standard curve at a first temperature rise rate or a crude oil combustion standard curve at different temperature rise rates; preparing an oil sand combustion sample to be detected by using the oil sand to be detected, and further performing a combustion test at a first heating rate to obtain the total amount of carbon monoxide and carbon dioxide generated by combustion of the oil sand combustion sample to be detected; determining the oil amount in the oil sand combustion sample to be detected by utilizing a crude oil combustion standard curve at a first temperature rising rate or crude oil combustion standard curves at different temperature rising rates based on the total amount of carbon monoxide and carbon dioxide generated by combustion of the oil sand combustion sample to be detected; determining the oil content of the oil sand to be tested: and determining the oil content of the oil sand to be detected by using the oil amount in the oil sand combustion sample to be detected.

Description

A kind of method for measuring oil content of oil sand

technical field

The invention belongs to the technical field of petroleum industry, and relates to a method for measuring oil content of oil sand.

Background technique

The distribution of remaining oil in the process of oilfield development is the key basis for the adjustment of development plans and enhanced oil recovery, and it is also an important parameter for indoor physical model experiment research.

At present, the commonly used methods for determining the oil content of oil sands mainly include: solvent extraction method and nuclear magnetic resonance method. The solvent extraction method is based on the principle of similar compatibility. The crude oil in the oil sand sample is extracted with a solvent under the condition of heating and refluxing, and the oil content of the sample is obtained by using the difference in the quality of the sample after extraction. The choice has a large impact on the determination of oil content. The nuclear magnetic resonance method uses nuclear magnetic resonance technology to measure the oil content. The principle is to use the nuclear magnetic resonance phenomenon of hydrogen atoms in the sample to quickly test the oil content of the sample. The results have a big impact.

In view of this, it is necessary to propose a low-cost and rapid new method for determining the oil content of oil sands.

SUMMARY OF THE INVENTION

The purpose of the present invention is to provide a low-cost and rapid method for determining the oil content of oil sands.

In order to achieve the above object, the present invention provides a method for measuring oil content of oil sands, wherein the method comprises:

Steps for establishing the standard curve: by using the oil sand standard samples with known different oil contents as combustion samples to carry out the combustion test, obtain the total amount of carbon monoxide and carbon dioxide generated by the combustion of the oil sand standard samples with different oil contents, and then obtain the first heating rate The crude oil combustion standard curve under different heating rates or the crude oil combustion standard curve under different heating rates; wherein, the crude oil combustion standard curve under a certain heating rate is the amount of combustion oil and the total amount of carbon monoxide and carbon dioxide generated by combustion when the heating rate is burned. the relationship curve;

Combustion determination step: use the oil sand to be tested to prepare the oil sand combustion sample to be tested, use the oil sand combustion sample to be tested to carry out the combustion test at the first heating rate, and obtain the carbon monoxide and carbon dioxide generated by the combustion of the oil sand combustion sample to be tested. total;

The step of determining the amount of combustion oil: based on the total amount of carbon monoxide and carbon dioxide produced by the combustion of the oil sand combustion sample to be tested, using the crude oil combustion standard curve under the first heating rate or the crude oil combustion standard curve under the different heating rates, Determine the amount of oil in the oil sand burning sample to be tested;

The step of determining the oil content of the oil sand to be tested: the oil content of the oil sand to be tested is determined by the oil content in the combustion sample of the oil sand to be tested.

In the above method, preferably, the standard curve establishment step includes at least one of Mode A, Mode B, Mode C, and Mode D;

Method A includes:

Use oil sand standard samples with known different oil contents as combustion samples to carry out the combustion test at the first heating rate to obtain the total amount of carbon monoxide and carbon dioxide produced by the combustion of oil sand standard samples with known different oil contents;

Based on the amount of oil in the known oil sand standard samples with different oil contents and the total amount of carbon monoxide and carbon dioxide produced by the combustion of the known oil sand standard samples with different oil contents, the combustion oil amount and the combustion at the first heating rate are obtained. The relationship curve between the generated carbon monoxide and the total amount of carbon dioxide is the crude oil combustion standard curve under the first heating rate;

Mode B includes:

The oil sand standard samples with known different oil contents were used as combustion samples to carry out the combustion test at the second heating rate, and the total amount of carbon monoxide and carbon dioxide produced by the combustion of the oil sand standard samples with known different oil contents was obtained; The first heating rate is different;

Based on the amount of oil in the known oil sand standard samples with different oil contents and the total amount of carbon monoxide and carbon dioxide produced by the combustion of the known oil sand standard samples with different oil contents, the combustion oil amount and the combustion oil amount when the combustion is carried out at the second heating rate are obtained. The relationship curve between the generated carbon monoxide and the total amount of carbon dioxide is the crude oil combustion standard curve under the second heating rate;

Using the first oil sand standard sample with known oil content as a combustion sample to carry out a combustion test at a first heating rate, to obtain the total amount of carbon monoxide and carbon dioxide produced by the combustion of the first oil sand standard sample with known oil content;

Based on the oil content in the oil sand standard sample with the first known oil content, the total amount of carbon monoxide and carbon dioxide produced by the combustion of the oil sand standard sample with the known oil content, and the crude oil combustion standard curve at the second heating rate, obtain The crude oil combustion standard curve under the first heating rate; wherein, the crude oil combustion standard curve under the first heating rate is obtained by shifting the crude oil combustion standard curve under the second heating rate upward or downward;

Mode C includes:

Use oil sand standard samples with known different oil contents as combustion samples to carry out combustion tests at different heating rates, and obtain the total amount of carbon monoxide and carbon dioxide produced by the combustion of oil sand standard samples with known different oil contents at different heating rates;

Based on the amount of oil in the oil sand standard samples with known different oil contents used for combustion at each heating rate and the total amount of carbon monoxide and carbon dioxide produced by the combustion of oil sand standard samples with known different oil contents at the heating rate, the The relationship curve between the amount of combustion oil and the total amount of carbon monoxide and carbon dioxide generated by combustion when each heating rate is burned is the standard curve of crude oil combustion at each heating rate;

Mode D includes:

Oil sand standard samples with known different oil contents were used as combustion samples to conduct combustion tests at the third heating rate to obtain the total amount of carbon monoxide and carbon dioxide produced by the combustion of oil sand standard samples with known different oil contents; the third heating rate was related to The first heating rate and the second heating rate may be the same or different;

Based on the amount of oil in the known oil sand standard samples with different oil contents and the total amount of carbon monoxide and carbon dioxide generated by the combustion of the known oil sand standard samples with different oil contents, the combustion oil amount and the combustion at the third heating rate are obtained. The relationship curve between the generated carbon monoxide and the total amount of carbon dioxide is the crude oil combustion standard curve at the third heating rate;

Use an oil sand standard sample with known oil content as a combustion sample to conduct combustion tests at different heating rates to obtain the total amount of carbon monoxide and carbon dioxide produced by the combustion of oil sand standard samples with known oil content at different heating rates;

Based on the amount of oil in the oil sand standard samples with known oil content used in the combustion test at different heating rates, the combustion of the oil sand standard samples with known oil content at each heating rate when the combustion test is performed at different heating rates The total amount of carbon monoxide and carbon dioxide produced and the standard curve of crude oil combustion at the second heating rate, respectively, obtain the relationship curve between the amount of combustion oil and the total amount of carbon monoxide and carbon dioxide generated by combustion when each heating rate is burned, that is, the curve at each heating rate. Crude oil combustion standard curve; wherein, the crude oil combustion standard curve at each temperature rate of combustion at different heating rates is obtained by shifting the crude oil combustion standard curve under a third heating rate upward or downward;

When constructing the standard curves of crude oil combustion under different heating rates, considering the influence of evaporation effect on combustion experiments, the standard curves under different heating rates are given, which can realize the prediction of oil content under various heating rates.

In the above method, preferably, the crude oil combustion standard curve under each heating rate is a straight line.

In the above method, preferably, the combustion device used in the combustion test includes a detachable connection between the combustion pool body and the upper end cover, the upper end cover is provided with a first through hole, the bottom surface of the combustion pool body is provided with a second through hole, and the combustion pool body is provided with a second through hole. Used to hold burning samples;

More preferably, the second through hole is used for gas injection, and the first through hole is used for gas discharge;

In a specific embodiment, the combustion device is performed by using the combustion pool body disclosed in FIG. 2 of the accompanying drawing in the patent application publication CN104122295A.

In the above method, preferably, each combustion test is carried out using the same combustion device at the same pressure and air injection rate.

In the above method, preferably, the combustion test is carried out in the following manner:

Load the combustion sample into the combustion device to complete the sample loading of the combustion device, and heat the combustion device at a certain heating rate under the condition of injecting air until the temperature reaches the rated temperature and stop heating; record the carbon monoxide and oxidation of the exhaust gas during the heating process. carbon concentration curve;

Obtain the total amount of carbon monoxide and carbon dioxide produced by combustion based on the concentration change curve of carbon monoxide and carbon dioxide in the exhaust gas during the heating process;

More preferably, the total amount of carbon monoxide and carbon dioxide produced by the combustion is obtained by integrating the concentration change curves of carbon monoxide and carbon dioxide in the exhaust gas during the heating process, wherein the integration is performed by the following formula:

为燃烧产生的一氧化碳与二氧化碳的总量，mol；q为燃烧试验中空气注入速度，L/min；

为燃烧试验中加热过程中排出气体的一氧化碳和二氧化碳的实测瞬时体积浓度值，％；其中22.4的单位为气体摩尔体积，单位为L/mol；In the formula,

is the total amount of carbon monoxide and carbon dioxide produced by combustion, mol; q is the air injection rate in the combustion test, L/min;

is the measured instantaneous volume concentration of carbon monoxide and carbon dioxide in the exhaust gas during the heating process in the combustion test, %; the unit of 22.4 is the gas molar volume, and the unit is L/mol;

More preferably, the loading of the combustion device includes:

Lay the first partition at the bottom to prevent sand leaking into the lower gas pipeline; lay the bottom sand layer on the stainless steel screen; lay the combustion sample layer on the bottom sand layer; lay the top sand layer on the combustion sample layer; A second compartment is laid on top of the layer;

Wherein, the first interlayer is preferably multi-layer stainless steel screen; the second interlayer is preferably ceramic wool;

More preferably, the combustion device is purged with nitrogen and/or air before sample loading.

In the above method, preferably, the crude oil in the oil sand standard sample with known oil content is the same as the crude oil in the oil sand to be tested.

In the above method, preferably, the weight ratio of crude oil to sand in the oil sand standard sample with known oil content is 0.4:10-0.8:10;

In a specific embodiment, the weight ratio of crude oil to sand in the oil sand standard sample with known oil content is 0.4:10, 0.5:10, 0.6:10, 0.7:10 or 0.8:10;

In a specific embodiment, the weight ratios of crude oil and sand in the oil sand standard samples with known different oil contents are 0.4:10, 0.5:10, 0.6:10, 0.7:10, and 0.8:10, respectively.

In the above method, preferably, the heating rate is 2.92°C/min-4.20°C/min;

In a specific embodiment, the heating rate is 2.92°C/min, 3.20°C/min, 3.62°C/min or 4.20°C/min;

In a specific embodiment, the different heating rates are 2.92°C/min, 3.20°C/min, 3.62°C/min, and 4.20°C/min, respectively.

In the above method, preferably, the method includes:

The total amount of carbon monoxide and carbon dioxide produced by the combustion of oil sand standard samples with different oil contents is obtained by using oil sand standard samples with known different oil contents as combustion samples for combustion test, and then the crude oil combustion standard curves under different heating rates are obtained. ; wherein, the standard curve of crude oil combustion under a certain heating rate is the relationship curve between the amount of combustion oil and the total amount of carbon monoxide and carbon dioxide generated by combustion when burning at the heating rate;

Use the oil sand to be tested to prepare the oil sand combustion sample to be tested, use the oil sand combustion sample to be tested to carry out the combustion test at different heating rates, and obtain the total amount of carbon monoxide and carbon dioxide produced by the combustion of the oil sand combustion sample to be tested;

Based on the total amount of carbon monoxide and carbon dioxide produced by the combustion of the oil sand combustion sample to be tested at different heating rates including the first heating rate, and using the crude oil combustion standard curves at the different heating rates, determine the corresponding heating rate at each heating rate. The amount of oil in the oil sand burning sample to be tested;

Determine the oil content of the oil sand to be tested by using the oil content in the combustion sample of the oil sand to be tested corresponding to each heating rate;

In a specific embodiment, determining the oil content of the oil sand to be tested by using the oil content in the combustion sample of the oil sand to be tested corresponding to each heating rate includes:

Based on the oil content in the combustion sample of the oil sand to be tested corresponding to each heating rate, determine the oil content of the oil sand to be tested corresponding to each heating rate;

Determine the oil content of the oil sand to be measured based on the oil content of the oil sand to be measured corresponding to each heating rate; for example, the oil content of the oil sand to be measured corresponding to each heating rate can be averaged as the oil content of the oil sand to be measured;

In this preferred technical scheme, considering the influence of evaporation effect on the combustion experiment, standard curves under different heating rates are given, so as to realize the prediction of oil content under various heating rate conditions.

The technical scheme provided by the invention corresponds to the oil content of the oil sand and the total amount of CO+CO ₂ produced by the combustion of crude oil, establishes a relationship curve between the two through a combustion test, that is, a standard curve of crude oil combustion, and obtains the target oil sand by the combustion test. The total amount of CO+CO ₂ was compared with the standard curve of crude oil combustion to obtain the oil content of the target oil sands. The technical scheme provided by the invention can effectively and quickly measure the oil content of the oil sand, and provide important physical parameters for the laboratory experimental research of the oil reservoir.

Description of drawings

FIG. 1 is a schematic diagram of the combustion apparatus used in Example 1. FIG.

FIG. 2 is a schematic diagram showing the concentration change curves of carbon monoxide and carbon oxide in the exhaust gas obtained in the heating process obtained in Example 1. FIG.

FIG. 3 is a graph showing the standard curve of crude oil combustion at a heating rate of 3.2° C./min in Example 1. FIG.

FIG. 4 is a graph showing the relationship between heating rate and gas production in Example 1. FIG.

FIG. 5 is a standard curve diagram of crude oil combustion under different heating rates in Example 1. FIG.

6 is a comparison diagram of the measured value and the measured value of the total amount of CO+CO ₂ produced by combustion under the heating rate of the oil sand to be tested in Example 1.

Detailed ways

To make the objectives, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are some, but not all, embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

burner

The combustion device used in Example 1 and Example 2 is shown in Figure 1. The combustion device includes a detachable connection to a combustion pool body 2 and an upper end cover 1; wherein, the open end of the combustion pool body 2 is provided with a lower flange, and the upper end cover 1. There is an upper flange. The connection between the combustion pool body 2 and the upper end cover 1 is realized by connecting the upper flange and the lower flange with bolts. When the upper flange and the lower flange are connected by bolts, the upper flange and the lower flange are connected by bolts. A red copper gasket is provided between the blue and blue for sealing; the upper end cover 1 is provided with a first through hole 11 , and the bottom surface of the combustion pool body 2 is provided with a second through hole 21 , and the combustion pool body 2 is used for holding combustion samples.

Example 1

The present embodiment provides a method for measuring the oil content of oil sands, comprising the following steps:

Step 1: Use oil sand standard samples with known different oil contents as combustion samples to conduct a combustion test at a heating rate of 3.2 °C/min to obtain the total amount of carbon monoxide and carbon dioxide generated by the combustion of oil sand standard samples with different oil contents, and then Obtain the crude oil combustion standard curve at a heating rate of 3.2 °C/min; wherein, the crude oil combustion standard curve at a certain heating rate is the relationship curve between the amount of combustion oil and the total amount of carbon monoxide and carbon dioxide generated by combustion when the heating rate is carried out. ; specifically:

1.1. Prepare oil sand standard samples with oil sand mass ratios of 0.4:10, 0.5:10, 0.6:10, 0.7:10, 0.8:10, respectively, and record them as the first oil sand standard sample and the second oil sand standard sample in turn , the third oil sand standard sample, the fourth oil sand standard sample, the fifth oil sand standard sample;

After pickling, washing and drying the 40-60 mesh quartz sand, weigh 0.40 g of crude oil and 10.00 g of the treated quartz sand with a one-thousandth balance, and mix the two evenly to obtain the first oil. Sand, weigh 4.50g of the first oil sand as the first oil sand standard sample;

After pickling, washing and drying the 40-60 mesh quartz sand, weigh 0.50 g of crude oil and 10.00 g of the treated quartz sand with a one-thousandth balance, and mix the two evenly to obtain the second oil. Sand, weigh 4.50g of the second oil sand as the second oil sand standard sample;

After pickling, washing and drying the 40-60 mesh quartz sand, weigh 0.60 g of crude oil and 10.00 g of the treated quartz sand with a one-thousandth balance, and mix the two evenly to obtain the third oil. Sand, weigh 4.50g of the third oil sand as the third oil sand standard sample;

After pickling, washing and drying the 40-60 mesh quartz sand, weigh 0.70 g of crude oil and 10.00 g of the treated quartz sand with a one-thousandth balance, and mix the two evenly to obtain the fourth oil. Sand, weigh 4.50g of the fourth oil sand as the fourth oil sand standard sample;

After pickling, washing and drying the 40-60 mesh quartz sand, weigh 0.80 g of crude oil and 10.00 g of the treated quartz sand with a one-thousandth balance, and mix the two evenly to obtain the fifth oil. Sand, weigh 4.50g of the fifth oil sand as the fifth oil sand standard sample;

1.2. Use the first oil sand standard sample, the second oil sand standard sample, the third oil sand standard sample, the fourth oil sand standard sample, and the fifth oil sand standard sample as combustion samples with a heating rate of 3.2°C/min Carry out a combustion test to obtain the total amount of carbon monoxide and carbon dioxide produced by the combustion of each oil sand standard sample; the details include:

1.2.1. Purge the combustion device with nitrogen or air, lay a multi-layer 200-mesh stainless steel screen at the bottom of the combustion pool body 2 as the first isolation layer, and lay 5g of quartz sand (40-60 g) on the first isolation layer. Objective Quartz sand, after pickling, water washing and drying treatment) as the bottom sand layer, lay the first oil sand standard sample (4.50g) on the bottom sand layer as the combustion sample layer, and lay 10g quartz on the combustion sample layer Sand (quartz sand of 40-60 mesh, after pickling, water washing and drying treatment) is used as the top sand layer, and ceramic wool is laid on the top sand layer as the second interlayer;

Fix the combustion pool body 2, clean the surface of the lower flange of the combustion pool body 2, put the copper washer into the upper groove of the lower flange, cover the upper end cover 1, and tighten the seal with bolts;

Put the installed combustion device into the heating furnace, and place it in the middle of the furnace, connect the pipeline, and check the air tightness of the combustion device; wherein, the first through hole 11 is connected with the exhaust pipe, and the second through hole 21 is connected with the intake pipe Connected, the exhaust pipe channel is connected with the gas analyzer, and the intake channel is connected with the gas flow meter;

Set the gas mass flow rate of the gas flowmeter to 1.0L/min, that is, the gas injection rate of the combustion device is 1.0L/min, first pass N ₂ for purging, wait for the O ₂ display of the gas analyzer to return to zero, and then turn on the compressed air , keep the flow rate at 1.0L/min, steadily increase the injection pressure to 1.0MPa and the back pressure to 0.5MPa, and wait for the readings of the gas flowmeter and gas analyzer to stabilize;

Set the heating furnace heating rate to 3.20℃/min, the temperature range to 25-550℃, press the control button to start heating;

When the temperature of the heating furnace reaches the specified temperature of 550 °C, the test is over, the heating is stopped, the upper and lower covers of the heating furnace are opened, and the combustion device is cooled down naturally;

Record the concentration change data and temperature data of carbon monoxide and carbon oxide obtained by the gas analyzer during the heating process, and then obtain the concentration change curve and temperature change curve of carbon monoxide and carbon oxide in the exhaust gas during the heating process (as shown in Figure 2) ;

Based on the concentration change curve of carbon monoxide and carbon dioxide in the exhaust gas during the heating process, the total amount of carbon monoxide and carbon dioxide produced by combustion is obtained; specifically, the integration is performed by the following formula:

为燃烧产生的一氧化碳与二氧化碳的总量，mol；q为燃烧试验中空气注入速度，L/min；

为燃烧试验中加热过程中排出气体的一氧化碳和二氧化碳的实测瞬时体积浓度值，％；In the formula,

is the total amount of carbon monoxide and carbon dioxide produced by combustion, mol; q is the air injection rate in the combustion test, L/min;

is the measured instantaneous volume concentration of carbon monoxide and carbon dioxide in the exhaust gas during the heating process in the combustion test, %;

The total amount of carbon monoxide and carbon dioxide produced by combustion is shown in Table 1;

1.2.2. Repeat step 1.2.1 to obtain the second oil sand standard sample as the combustion sample, and carry out the total amount of carbon monoxide and carbon dioxide produced by the combustion test at a heating rate of 3.2°C/min;

The only difference from step 1.2.1 is that the combustion sample layer loaded in the combustion device is the second oil sand standard sample (4.50g) instead of the first oil sand standard sample (4.50g);

The total amount of carbon monoxide and carbon dioxide produced by combustion is shown in Table 1;

1.2.3. Repeat step 1.2.1 to obtain the third oil sand standard sample as the combustion sample, and carry out the total amount of carbon monoxide and carbon dioxide produced by the combustion test at a heating rate of 3.2°C/min;

The only difference from step 1.2.1 is that the combustion sample layer loaded in the combustion device is the third oil sand standard sample (4.50g) instead of the first oil sand standard sample (4.50g);

The total amount of carbon monoxide and carbon dioxide produced by combustion is shown in Table 1;

1.2.4. Repeat step 1.2.1 to obtain the fourth oil sand standard sample as the combustion sample, and carry out the total amount of carbon monoxide and carbon dioxide produced by the combustion test at a heating rate of 3.2°C/min;

The only difference from step 1.2.1 is that the combustion sample layer loaded in the combustion device is the fourth oil sand standard sample (4.50g) instead of the first oil sand standard sample (4.50g);

The total amount of carbon monoxide and carbon dioxide produced by combustion is shown in Table 1;

1.2.5. Repeat step 1.2.1 to obtain the fifth oil sand standard sample as the combustion sample, and carry out the total amount of carbon monoxide and carbon dioxide produced by the combustion test at a heating rate of 3.2°C/min;

The only difference from step 1.2.1 is that the combustion sample layer loaded in the combustion device is the fifth oil sand standard sample (4.50g) instead of the first oil sand standard sample (4.50g);

The total amount of carbon monoxide and carbon dioxide produced by combustion is shown in Table 1;

1.3. Based on the amount of oil in each oil sand standard sample and the total amount of carbon monoxide and carbon dioxide produced by the combustion of each oil sand standard sample obtained in step 1.2 (see Table 1), obtain the combustion at a heating rate of 3.20°C/min. The relationship curve between the amount of oil and the total amount of carbon monoxide and carbon dioxide produced by combustion is the standard curve of crude oil combustion at a heating rate of 3.20°C/min;

The results are shown in Figure 3;

Table 1

Step 2: Obtain the oil sand combustion sample to be tested; specifically,

After pickling, washing and drying the 40-60 mesh quartz sand, weigh 7.00g of the treated quartz sand with a one-thousandth balance; weigh 3.00g of the oil sand to be tested; mix the two evenly And weigh 4.50g as the oil sand burning sample to be tested.

Step 3: Use the oil sand combustion sample to be tested to conduct a combustion test at a heating rate of 3.20°C/min, and obtain the total amount of carbon monoxide and carbon dioxide generated by the combustion of the oil sand combustion sample to be tested; specifically,

Repeat step 1.2.1 to obtain the oil sand combustion sample to be tested as the total amount of carbon monoxide and carbon dioxide produced by the combustion test at a heating rate of 3.2 °C/min;

The only difference from step 1.2.1 is that the combustion sample layer loaded in the combustion device is the oil sand combustion sample to be tested (4.50g) instead of the first oil sand standard sample (4.50g);

The total amount of carbon monoxide and carbon dioxide produced by combustion is shown in Table 2;

Step 4: Based on the total amount of carbon monoxide and carbon dioxide produced by the combustion of the oil sand combustion sample to be tested, the crude oil combustion standard curve at a heating rate of 3.2 °C/min is used to determine the amount of oil in the oil sand combustion sample to be tested; In terms of:

Based on the total amount of carbon monoxide and carbon dioxide produced by the combustion of the oil sand combustion sample to be tested, the crude oil combustion standard curve at a heating rate of 3.2°C/min is used to determine the amount of oil in the oil sand combustion sample to be tested;

The oil content of the oil sand to be tested is determined based on the oil content in the combustion sample of the oil sand to be tested; specifically, the following formula is used to determine the oil content of the oil sand to be tested:

In the formula, m is the amount of oil in the combustion sample of the oil sand to be tested, g; M is the oil content of the oil sand to be tested, %;

The results are shown in Table 2.

Table 2

Example 2

The present embodiment provides a method for measuring the oil content of oil sands, comprising the following steps:

Step 1: Use oil sand standard samples with known different oil contents as combustion samples to carry out combustion test, obtain the total amount of carbon monoxide and carbon dioxide produced by the combustion of oil sand standard samples with different oil contents, and then obtain the combustion of crude oil under different heating rates Standard curve; wherein, the standard curve of crude oil combustion under a certain heating rate is the relationship curve between the amount of combustion oil and the total amount of carbon monoxide and carbon dioxide generated by the combustion when burning at the heating rate; specifically, it includes:

Carry out steps 1.1-1.2 of this embodiment in the same manner as steps 1.1-1.2 in embodiment 1;

1.1. Prepare oil sand standard samples with oil sand mass ratios of 0.4:10, 0.5:10, 0.6:10, 0.7:10, 0.8:10, respectively, and record them as the first oil sand standard sample and the second oil sand standard sample in turn , the third oil sand standard sample, the fourth oil sand standard sample, the fifth oil sand standard sample;

After pickling, washing and drying the 40-60 mesh quartz sand, weigh 0.40 g of crude oil and 10.00 g of the treated quartz sand with a one-thousandth balance, and mix the two evenly to obtain the first oil. Sand, weigh 4.50g of the first oil sand as the first oil sand standard sample;

After pickling, washing and drying the 40-60 mesh quartz sand, weigh 0.50 g of crude oil and 10.00 g of the treated quartz sand with a one-thousandth balance, and mix the two evenly to obtain the second oil. Sand, weigh 4.50g of the second oil sand as the second oil sand standard sample;

After pickling, washing and drying the 40-60 mesh quartz sand, weigh 0.60 g of crude oil and 10.00 g of the treated quartz sand with a one-thousandth balance, and mix the two evenly to obtain the third oil. Sand, weigh 4.50g of the third oil sand as the third oil sand standard sample;

After pickling, washing and drying the 40-60 mesh quartz sand, weigh 0.70 g of crude oil and 10.00 g of the treated quartz sand with a one-thousandth balance, and mix the two evenly to obtain the fourth oil. Sand, weigh 4.50g of the fourth oil sand as the fourth oil sand standard sample;

After pickling, washing and drying the 40-60 mesh quartz sand, weigh 0.80 g of crude oil and 10.00 g of the treated quartz sand with a one-thousandth balance, and mix the two evenly to obtain the fifth oil. Sand, weigh 4.50g of the fifth oil sand as the fifth oil sand standard sample;

1.2. Use the first oil sand standard sample, the second oil sand standard sample, the third oil sand standard sample, the fourth oil sand standard sample, and the fifth oil sand standard sample as combustion samples with a heating rate of 3.2°C/min Carry out a combustion test to obtain the total amount of carbon monoxide and carbon dioxide produced by the combustion of each oil sand standard sample; the details include:

1.2.1. Purge the combustion device with nitrogen or air, lay a multi-layer 200-mesh stainless steel screen at the bottom of the combustion pool body 2 as the first isolation layer, and lay 5g of quartz sand (40-60 g) on the first isolation layer. Objective Quartz sand, after pickling, water washing and drying treatment) as the bottom sand layer, lay the first oil sand standard sample (4.50g) on the bottom sand layer as the combustion sample layer, and lay 10g quartz on the combustion sample layer Sand (quartz sand of 40-60 mesh, after pickling, water washing and drying treatment) is used as the top sand layer, and ceramic wool is laid on the top sand layer as the second interlayer;

Fix the combustion pool body 2, clean the surface of the lower flange of the combustion pool body 2, put the copper washer into the upper groove of the lower flange, cover the upper end cover 1, and tighten the seal with bolts;

Put the installed combustion device into the heating furnace, and place it in the middle of the furnace, connect the pipeline, and check the air tightness of the combustion device; wherein, the first through hole 11 is connected with the exhaust pipe, and the second through hole 21 is connected with the intake pipe Connected, the exhaust pipe channel is connected with the gas analyzer, and the intake channel is connected with the gas flow meter;

Set the gas mass flow rate of the gas flowmeter to 1.0L/min, that is, the gas injection rate of the combustion device is 1.0L/min, first pass N ₂ for purging, wait for the O ₂ display of the gas analyzer to return to zero, and then turn on the compressed air , keep the flow rate at 1.0L/min, steadily increase the injection pressure to 1.0MPa and the back pressure to 0.5MPa, and wait for the readings of the gas flowmeter and gas analyzer to stabilize;

Set the heating furnace heating rate to 3.20℃/min, the temperature range to 25-550℃, press the control button to start heating;

When the temperature of the heating furnace reaches the specified temperature of 550 °C, the test is over, the heating is stopped, the upper and lower covers of the heating furnace are opened, and the combustion device is cooled down naturally;

Record the concentration change data and temperature data of carbon monoxide and carbon oxide obtained by the gas analyzer during the heating process, and then obtain the concentration change curve and temperature change curve of carbon monoxide and carbon oxide in the exhaust gas during the heating process (as shown in Figure 2) ;

Based on the concentration change curve of carbon monoxide and carbon dioxide in the exhaust gas during the heating process, the total amount of carbon monoxide and carbon dioxide produced by combustion is obtained; specifically, the integration is performed by the following formula:

In the formula, n _co+co2 is the total amount of carbon monoxide and carbon dioxide produced by combustion, mol; q is the air injection rate in the combustion test, L/min; C _CO+CO2 is the carbon monoxide and carbon dioxide in the exhaust gas during the heating process in the combustion test. The measured instantaneous volume concentration value, %;

The total amount of carbon monoxide and carbon dioxide produced by combustion is shown in Table 1;

1.2.2. Repeat step 1.2.1 to obtain the second oil sand standard sample as the combustion sample, and carry out the total amount of carbon monoxide and carbon dioxide produced by the combustion test at a heating rate of 3.2°C/min;

The only difference from step 1.2.1 is that the combustion sample layer loaded in the combustion device is the second oil sand standard sample (4.50g) instead of the first oil sand standard sample (4.50g);

The total amount of carbon monoxide and carbon dioxide produced by combustion is shown in Table 1;

1.2.3. Repeat step 1.2.1 to obtain the third oil sand standard sample as the combustion sample, and carry out the total amount of carbon monoxide and carbon dioxide produced by the combustion test at a heating rate of 3.2°C/min;

The only difference from step 1.2.1 is that the combustion sample layer loaded in the combustion device is the third oil sand standard sample (4.50g) instead of the first oil sand standard sample (4.50g);

The total amount of carbon monoxide and carbon dioxide produced by combustion is shown in Table 1;

1.2.4. Repeat step 1.2.1 to obtain the fourth oil sand standard sample as the combustion sample, and carry out the total amount of carbon monoxide and carbon dioxide produced by the combustion test at a heating rate of 3.2°C/min;

The only difference from step 1.2.1 is that the combustion sample layer loaded in the combustion device is the fourth oil sand standard sample (4.50g) instead of the first oil sand standard sample (4.50g);

The total amount of carbon monoxide and carbon dioxide produced by combustion is shown in Table 1;

1.2.5. Repeat step 1.2.1 to obtain the fifth oil sand standard sample as the combustion sample, and carry out the total amount of carbon monoxide and carbon dioxide produced by the combustion test at a heating rate of 3.2°C/min;

The only difference from step 1.2.1 is that the combustion sample layer loaded in the combustion device is the fifth oil sand standard sample (4.50g) instead of the first oil sand standard sample (4.50g);

The total amount of carbon monoxide and carbon dioxide produced by combustion is shown in Table 1;

1.3. Based on the amount of oil in each oil sand standard sample and the total amount of carbon monoxide and carbon dioxide produced by the combustion of each oil sand standard sample obtained in step 1.2 (see Table 1), obtain the combustion at a heating rate of 3.20°C/min. The relationship curve between the amount of oil and the total amount of carbon monoxide and carbon dioxide produced by combustion is the standard curve of crude oil combustion at a heating rate of 3.20°C/min;

The results are shown in Figure 5;

1.4. Use the third oil sand standard sample as the combustion sample to carry out the combustion test at the temperature rate of 2.92°C/min, 3.62°C/min, 4.2°C/min, and obtain the oil sand standard sample combustion with known oil content at each heating rate. The total amount of carbon monoxide and carbon dioxide produced (see Figure 4 for results); specifically:

1.4.1. Repeat step 1.2.3 to obtain the third oil sand standard sample as the combustion sample, and carry out the total amount of carbon monoxide and carbon dioxide produced by the combustion test at a heating rate of 2.92°C/min;

The only difference from step 1.2.1 is that the heating rate is 2.92°C/min instead of 3.2°C/min;

The total amount of carbon monoxide and carbon dioxide produced by combustion is shown in Table 3;

1.4.2. Repeat step 1.2.3 to obtain the third oil sand standard sample as the combustion sample, and carry out the total amount of carbon monoxide and carbon dioxide produced by the combustion test at a heating rate of 3.62°C/min;

The only difference from step 1.2.1 is that the heating rate is 3.62°C/min instead of 3.2°C/min;

The total amount of carbon monoxide and carbon dioxide produced by combustion is shown in Table 3;

1.4.3. Repeat step 1.2.3 to obtain the third oil sand standard sample as the combustion sample, and carry out the total amount of carbon monoxide and carbon dioxide produced by the combustion test at a heating rate of 4.2°C/min;

The only difference from step 1.2.1 is that the heating rate is 4.2°C/min instead of 3.2°C/min;

The total amount of carbon monoxide and carbon dioxide produced by combustion is shown in Table 3;

table 3

1.5. Based on the amount of oil in the third oil sand standard sample, the total amount of carbon monoxide and carbon dioxide produced by the combustion of the third oil sand standard sample at each heating rate obtained in step 1.4, and the crude oil combustion standard curve at a heating rate of 3.20°C/min , obtain the relationship curve between the amount of combustion oil and the total amount of carbon monoxide and carbon dioxide generated by combustion when the heating rate is 2.92°C/min, 3.62°C/min, 4.2°C/min, namely 2.92°C/min, 3.62°C/min, 4.2°C The crude oil combustion standard curve at the heating rate of 2.92°C/min, 3.62°C/min, 4.2°C/min and the crude oil combustion standard curve at the heating rate of 3.20°C/min are combined to form different heating rates The crude oil combustion standard curve at the heating rate, the results are shown in Figure 5; among them, the crude oil combustion standard curve at the heating rate of 2.92°C/min, 3.62°C/min, and 4.2°C/min The standard curve is shifted up or down.

Step 2: Obtain the oil sand combustion sample to be tested; specifically,

In this example, in order to better know the accuracy of the technical solution, a standard oil sand sample was used as the oil sand combustion sample to be tested; specifically,

After pickling, washing and drying the 40-60 mesh quartz sand, weigh 0.50 g of crude oil and 10.00 g of the treated quartz sand with a one-thousandth balance, and mix the two evenly to obtain the oil to be tested. Sand, weigh 4.50g of the oil sand to be tested as the standard sample of the oil sand for geological survey;

Step 3: use the oil sand combustion sample to be tested to carry out a combustion test at a heating rate of 3.20°C/min, to obtain the total amount of carbon monoxide and carbon dioxide generated by the combustion of the oil sand combustion sample to be tested;

Step 3: Use the oil sand combustion sample to be tested to carry out the combustion test at the heating rate of 2.92°C/min,: 3.62°C/min, 4.2°C/min, and obtain 2.92°C/min, 3.20°C/min, 3.62°C/min, 4.2°C The total amount of carbon monoxide and carbon dioxide produced by the combustion of the oil sand combustion sample to be tested at a heating rate of ℃/min; specifically,

3.1. Repeat step 1.2.1 to obtain the oil sand combustion sample to be tested as the total amount of carbon monoxide and carbon dioxide produced by the combustion test at a heating rate of 2.92°C/min;

The only difference from step 1.2.1 is that the combustion sample layer loaded in the combustion device is the oil sand combustion sample to be tested (4.50g) instead of the first oil sand standard sample (4.50g); the heating rate is 2.92℃/ min instead of 3.2°C/min;

The total amount of carbon monoxide and carbon dioxide produced by combustion is shown in Table 4;

3.2. Repeat step 3.1 to obtain the oil sand combustion sample to be tested as the total amount of carbon monoxide and carbon dioxide produced by the combustion test at a heating rate of 3.62°C/min;

The only difference from step 3.1 is that the heating rate is 3.62°C/min instead of 2.92°C/min;

3.3. Repeat step 3.1 to obtain the oil sand combustion sample to be tested as the combustion sample, and the total amount of carbon monoxide and carbon dioxide produced by the combustion test at a heating rate of 4.2°C/min;

The only difference from step 3.1 is that the heating rate is 4.2°C/min instead of 2.92°C/min;

The total amount of carbon monoxide and carbon dioxide produced by combustion is shown in Table 4;

Step 4: Based on the total amount of carbon monoxide and carbon dioxide produced by the combustion of the oil sand combustion sample to be tested, and using the crude oil combustion standard curves under different heating rates, determine the oil amount in the oil sand combustion sample to be tested; specifically:

Based on the total amount of carbon monoxide and carbon dioxide produced by the combustion of the corresponding oil sand combustion samples under each heating rate, the oil sand combustion samples to be tested corresponding to each heating rate were determined using the crude oil combustion standard curves at different heating rates. the amount of oil in;

Based on the oil content in the combustion sample of the oil sand to be tested corresponding to each heating rate, the oil content of the oil sand to be tested corresponding to each heating rate is determined;

The oil content of the oil sand to be tested is determined based on the oil content of the oil sand to be tested corresponding to each heating rate.

Table 4

Accuracy analysis: According to the actual oil amount and the total amount of carbon monoxide and carbon dioxide produced by combustion at different heating rates, the oil sand combustion samples to be tested are put on the standard curve of crude oil combustion at different heating rates. The results are shown in Figure 6. Show. It can be seen from Figure 6 that the combustion results of the oil sand combustion samples to be tested at different heating rates are in good agreement with the crude oil combustion standard curves at different heating rates. The relative errors are shown in Table 4, indicating that this method can predict oil under different heating rates. Sand oil content is feasible and reliable.

Claims (10)

1. A method for determining oil content in oil sands, wherein the method comprises:

and (3) standard curve establishing: carrying out a combustion test by using oil sand standard samples with different known oil contents as combustion samples to obtain the total amount of carbon monoxide and carbon dioxide generated by the combustion of the oil sand standard samples with different oil contents, and further obtaining a crude oil combustion standard curve at a first temperature rise rate or a crude oil combustion standard curve at different temperature rise rates; wherein, the crude oil combustion standard curve at a certain heating rate is a relation curve of the combustion oil quantity and the total quantity of carbon monoxide and carbon dioxide generated by combustion when combustion is carried out at the heating rate;

and (3) a combustion determination step: preparing an oil sand combustion sample to be detected by using oil sand to be detected, and performing a combustion test by using the oil sand combustion sample to be detected at a first heating rate to obtain the total amount of carbon monoxide and carbon dioxide generated by combustion of the oil sand combustion sample to be detected;

a combustion oil amount determining step: determining the oil amount in the oil sand combustion sample to be detected by utilizing the crude oil combustion standard curve at the first temperature rising rate or the crude oil combustion standard curves at different temperature rising rates on the basis of the total amount of carbon monoxide and carbon dioxide generated by combustion of the oil sand combustion sample to be detected;

determining the oil content of the oil sand to be tested: and determining the oil content of the oil sand to be detected by using the oil amount in the oil sand combustion sample to be detected.

2. The method of claim 1, wherein the standard curve establishing step comprises at least one of a mode a, a mode B, a mode C, a mode D;

the method A comprises the following steps:

carrying out a combustion test at a first temperature rise rate by using the oil sand standard samples with different known oil contents as combustion samples to obtain the total amount of carbon monoxide and carbon dioxide generated by the combustion of the oil sand standard samples with different known oil contents;

acquiring a relation curve of the combustion oil quantity and the total amount of carbon monoxide and carbon dioxide generated by combustion when the oil quantity is combusted at a first temperature-rising rate, namely a crude oil combustion standard curve at the first temperature-rising rate, based on the oil quantity in the oil sand standard samples with different known oil contents and the total amount of carbon monoxide and carbon dioxide generated by combustion of the oil sand standard samples with different known oil contents;

the mode B includes:

carrying out a combustion test at a second temperature rise rate by using the oil sand standard samples with different known oil contents as combustion samples to obtain the total amount of carbon monoxide and carbon dioxide generated by combustion of the oil sand standard samples with different known oil contents; the second temperature rise rate is different from the first temperature rise rate;

acquiring a relation curve of the combustion oil quantity and the total amount of carbon monoxide and carbon dioxide generated by combustion when the oil quantity is combusted at a second temperature-rising rate, namely a crude oil combustion standard curve at the second temperature-rising rate, based on the oil quantity in the oil sand standard samples with different known oil contents and the total amount of carbon monoxide and carbon dioxide generated by combustion of the oil sand standard samples with different known oil contents;

carrying out a combustion test at a first temperature rise rate by using the first oil sand standard sample with known oil content as a combustion sample to obtain the total amount of carbon monoxide and carbon dioxide generated by combustion of the first oil sand standard sample with known oil content;

acquiring a crude oil combustion standard curve at a first temperature rising rate based on the oil amount in the oil sand standard sample with the first known oil content, the total amount of carbon monoxide and carbon dioxide generated by combustion of the oil sand standard sample with the first known oil content and the crude oil combustion standard curve at a second temperature rising rate; the crude oil combustion standard curve at the first temperature rise rate is obtained by translating the crude oil combustion standard curve at the second temperature rise rate upwards or downwards;

the mode C comprises the following steps:

respectively using the oil sand standard samples with different known oil contents as combustion samples to perform combustion tests at different heating rates, and obtaining the total amount of carbon monoxide and carbon dioxide generated by the combustion of the oil sand standard samples with different known oil contents at different heating rates;

respectively acquiring a relation curve of the combustion oil amount and the total amount of carbon monoxide and carbon dioxide generated by combustion when combustion is carried out at each temperature rise rate, namely a crude oil combustion standard curve at each temperature rise rate, based on the oil amount in the oil sand standard samples with known different oil contents used for combustion at each temperature rise rate and the total amount of carbon monoxide and carbon dioxide generated by combustion of the oil sand standard samples with known different oil contents at the temperature rise rate;

the mode D includes:

carrying out a combustion test at a third temperature rise rate by using the oil sand standard samples with known different oil contents as combustion samples to obtain the total amount of carbon monoxide and carbon dioxide generated by combustion of the oil sand standard samples with known different oil contents; the third heating rate can be the same as or different from the first heating rate and the second heating rate;

acquiring a relation curve of the combustion oil quantity and the total amount of carbon monoxide and carbon dioxide generated by combustion when the oil quantity is combusted at a third temperature-rising rate, namely a crude oil combustion standard curve at the third temperature-rising rate, based on the oil quantity in the oil sand standard samples with different known oil contents and the total amount of carbon monoxide and carbon dioxide generated by combustion of the oil sand standard samples with different known oil contents;

respectively using an oil sand standard sample with known oil content as a combustion sample to perform combustion tests at different heating rates, and obtaining the total amount of carbon monoxide and carbon dioxide generated by the combustion of the oil sand standard sample with known oil content at different heating rates;

respectively obtaining a relation curve of the combustion oil amount and the total amount of carbon monoxide and carbon dioxide generated by combustion at each temperature rise rate, namely a crude oil combustion standard curve at each temperature rise rate, based on the oil amount in the oil sand standard sample with known oil content used for carrying out the combustion test at different temperature rise rates, the total amount of carbon monoxide and carbon dioxide generated by combustion of the oil sand standard sample with known oil content at each temperature rise rate when carrying out the combustion test at different temperature rise rates and a crude oil combustion standard curve at a second temperature rise rate; and the standard curve of the combustion of the crude oil at each temperature rate for combustion at different temperature rise rates is obtained by translating the standard curve of the combustion of the crude oil at a third temperature rise rate upwards or downwards.

3. The method according to claim 1 or 2, wherein the method comprises:

carrying out a combustion test by using oil sand standard samples with different known oil contents as combustion samples to obtain the total amount of carbon monoxide and carbon dioxide generated by the combustion of the oil sand standard samples with different oil contents, and further obtaining a crude oil combustion standard curve at different heating rates; wherein, the crude oil combustion standard curve at a certain heating rate is a relation curve of the combustion oil quantity and the total quantity of carbon monoxide and carbon dioxide generated by combustion when combustion is carried out at the heating rate;

preparing an oil sand combustion sample to be detected by using oil sand to be detected, and performing a combustion test by using the oil sand combustion sample to be detected at different heating rates to obtain the total amount of carbon monoxide and carbon dioxide generated by combustion of the oil sand combustion sample to be detected;

determining the oil amount in the oil sand combustion sample to be detected corresponding to each temperature rise rate by utilizing the crude oil combustion standard curve at different temperature rise rates based on the total amount of carbon monoxide and carbon dioxide generated by combustion of the oil sand combustion sample to be detected at different temperature rise rates including the first temperature rise rate;

and determining the oil content of the oil sand to be detected by using the oil amount in the corresponding oil sand combustion sample to be detected at each temperature rise rate.

4. The method of claim 3, wherein determining the oil content of the oil sand to be tested by using the oil amount in the corresponding oil sand combustion sample to be tested at each temperature rise rate comprises:

determining the oil content of the oil sand to be detected corresponding to each heating rate based on the oil amount in the corresponding oil sand combustion sample to be detected corresponding to each heating rate;

and determining the oil content of the oil sand to be detected based on the corresponding oil content of the oil sand to be detected at each heating rate.

5. The method of claim 1 or 2, wherein the standard curve for crude oil combustion at each ramp rate is a straight line.

6. A method according to claim 1 or claim 2, wherein each combustion test is carried out using the same combustion apparatus at the same pressure and air injection rate.

7. The method according to claim 1 or 2, wherein preferably the crude oil in the oil sands standard of known oil content is of the same composition as the crude oil in the oil sands to be tested.

8. The method according to claim 1 or 2, wherein the combustion device used in the combustion test comprises a combustion tank body and an upper end cover which are detachably connected, wherein the upper end cover is provided with a first through hole, the bottom surface of the combustion tank body is provided with a second through hole, and the combustion tank body is used for containing a combustion sample;

preferably, the second through hole is used for gas injection, and the first through hole is used for gas discharge.

9. The method of any of claims 1-8, wherein the burn test is performed by:

loading a combustion sample into a combustion device to finish the loading of the combustion device, heating the combustion device at a certain heating rate under the condition of injecting air, and stopping heating until the temperature is raised to a rated temperature; recording the concentration change curves of carbon monoxide and carbon oxide in the exhaust gas in the heating process;

and acquiring the total amount of the carbon monoxide and the carbon dioxide generated by combustion based on the concentration change curve of the carbon monoxide and the carbon dioxide of the exhaust gas in the heating process.

10. The method of claim 9, wherein,

the total amount of carbon monoxide and carbon dioxide produced by the combustion is obtained by integrating the concentration change curves of carbon monoxide and carbon dioxide in the exhaust gas during heating, wherein the integration is performed by the following formula:

in the formula (I), the compound is shown in the specification,

mol is the total amount of carbon monoxide and carbon dioxide generated by combustion; q is the air injection speed in the combustion test, L/min;

is the actually measured instantaneous volume concentration value,%, of carbon monoxide and carbon dioxide of the exhaust gas in the heating process in the combustion test;

the combustion apparatus sample loading comprises: laying a first interlayer at the bottom to prevent sand from leaking into a lower gas pipeline; laying a bottom sand layer on the stainless steel screen; paving a combustion sample layer on the bottom sand layer; laying a top sand layer on the combustion sample layer; laying a second interlayer on the top of the top sand layer; wherein, the first interlayer is a multi-layer stainless steel screen; the second interlayer is made of ceramic wool.

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