Master thesis in the field of chemical engineering
Abstract
Laboratory study of iron oxide production on a microstructure scale using the precipitation method with supercritical antisolvent
by:
One ??of the problems of cement used in oil wells, which are used to connect wall pipes and well walls, is that these cements do not have the desired resistance against high temperature and pressure. Therefore, at the high temperature and pressure of the well, cement cracks. One of the ways to make it resistant is to add some special additives in micrometer or nanometer size to cement and improve its resistance against pressure and temperature. In this project, an attempt is made to produce iron oxide as one of the cement additives by precipitation method with supercritical anti-solvent on a microstructural scale. Several parameters affect the quality and properties of the produced products, as well as increasing the efficiency and improving the performance of supercritical processes, among which we can mention the temperature, pressure and initial concentration of the solution.
In this research, 9 experiments were carried out under different conditions of concentration (1-5.6 mg/ml), temperature (K) (15.328-15.308), pressure (100-150 bar) and carbon dioxide flow rate. (25-75 mg/min) has been done and their effect on particle size and morphology has been investigated. In various laboratory conditions, particles with a diameter between 17.2 and 23.0 micrometers have been obtained. In addition, the results show that larger particles are formed by increasing the pressure. Finally, the optimum laboratory conditions are 120 load, temperature of 35 degrees Celsius and concentration of 1.5 mg/ml.
1- Preface
Today, the use of supercritical fluid technology to produce products with micro or nano sizes has increased. Due to some gas-type and liquid-type properties of supercritical fluids, such as high permeability and density, it is possible to use supercritical fluid processes in the production of various materials on a micro or nano scale in various industries. One of the important applications of such processes is the production of various substances such as drugs, proteins, biopolymers, as well as chemicals on a micro or nano scale.
The technology of using supercritical fluids provides numerous measures to achieve the mentioned goals. We know that carbon dioxide is one of the most widely used fluids in supercritical processes. Carbon dioxide has a critical pressure of about 73.8 bar and a critical temperature of 31.1 degrees Celsius. In addition, carbon dioxide is a non-toxic, non-flammable, cheap and environmentally friendly liquid. Until 1984, there was no reference to the use of supercritical fluid for the production of fine particles, until Krokonis [1] and his colleagues recorded good results for nucleation in other materials. Among the studies conducted, we can mention the reduction of the particle size of pharmaceutical materials and materials that are sensitive to high temperature processes.
One ??of the important methods in the production of materials in micro-nano sizes is the supercritical anti-solvent method using an organic solvent. It should be noted that in this method, the desired component is dissolved in an organic solvent in a supersaturated form, and then it comes into contact with a fluid such as carbon dioxide in supercritical or near-critical conditions.
The important point is that carbon dioxide dissolves well in most organic solvents, so when carbon dioxide is dissolved in an organic solvent, a supersaturated state occurs for the soluble component and causes the desired component to crystallize [1].
1-2-Nanotechnology and its application in the oil industry
Any type of process that takes place on atoms, molecules, semiconductors, solids and liquids on a scale below one hundred nanometers is called nanotechnology. Nanotechnology has many aspects. Although the dimensions in the nano scale are much smaller than millimeters and micrometers, but due to the proximity of the nano dimensions to the dimensions of nature, it is easier to work in this scale. Nanotechnology is currently transforming human life and has created a lot of changes in industries, and it is expected that this process will continue at a faster pace in the coming years. One of the fields in which nanotechnology has been introduced is the upstream oil industry, which, according to the definition, includes from exploration to before the refinery. Here, the use of nano particles and nano additives in the cementing of oil wells is examined.
During the drilling of wells, in order to stabilize the well wall and prevent the wall from collapsing, at certain intervals, pipes (wall pipes) are driven into the well, and the back of them is cemented, and the wall pipes are attached to the well wall by cement and fixed. This process is done in such a way that first the wall pipes are connected to each other and pushed to the end of the well. Then the cement is pumped from the bottom of the well to the back of the wall pipes (the space between the wall pipes and the well mouth) and rises to the ground level. Finally, the time required for the cement to dry is considered so that the wall pipes are connected to the well wall. From the moment of cement injection until its complete drying, the wall pipes are connected to the mast by cables. The cements used should have controllable setting properties, pumpability, viscosity, and final hardness, as well as suitable viscosity, strength, and setting time properties.
Using nano additives, these properties can be met. By adding nanoparticles to this cement, due to the properties between the quantum properties and the bulk properties of the material, they can create suitable properties. One of the prominent features of these particles is the same homogeneity of the whole mixture after adding, which causes homogenization of cement properties. NanoProduct Corp. has used calcium silicate nanoparticles in cement and the resulting cement can be used at high temperatures, so it can be a suitable option for deep oil wells and geothermal wells [2].
One ??of the problems of cement used in oil wells, which are used to connect wall pipes and well walls, is that these cements do not have the desired resistance against high temperature and pressure. Therefore, at the high temperature and pressure of the well, the cement cracks. One of the ways to make it resistant is to add some special additives in micrometer or nanometer size to cement and improve the compressive and bending strength and the resistance of cement against temperature. Nanoparticles added to cement can be of the type of compounds that make up cement itself (silica oxide, iron oxide, and alumina) and of other compounds, which are used to create specific properties in cement. For example, to obtain cement with suitable properties for use in oil wells, it is suitable to add nanoparticles. The main purpose of using nano additives in oil well wall cement is to deal with problems in terms of low tank pressure and the need to create the necessary pressure by the cement used.
In addition to the above, increasing compressive strength and reducing porosity and permeability and finally controlling and inhibiting gas and fluid migration from within the cement column are other advantages of using nanoparticles in the design of cement slurry.
Contents & References of Laboratory study of iron oxide production on a microstructural scale using precipitation method with supercritical antisolvent
List:
2
Chapter One: Introduction.
2
1-1- Preface ..
3
1-2- Nanotechnology and its application in the oil industry. .
4
1-3- Nanotechnology and oil well cement. .
4
1-4- Introduction of some nano additives used in cement. .
8
1-5- Definition of supercritical fluid. .
10
1-6- Advantages of extraction by supercritical fluid. .
11
1-7- Applications of supercritical technology. .
12
1-8- Application of supercritical processes in the production of fine particles. 14-1-8-1 RESS process. .
22
Chapter Two: Review of Past Research
37
Chapter Three: Pilot Test.
37
3-1- Fundamentals of Supercritical Extraction Pilot Design and Specifications.
38
3-2- Examining the Main Components of Supercritical Pilot.
38
3-2-1- Providing the test pressure.
39
3-2-2- Providing the test temperature.
39
3-2-3- The main container of the test.
39
3-2-4- Metal filter..
39
3-3- Designing the supercritical laboratory device.
40
3-3-1- main container..
42
3-3-2- metal filter..
43
3-3-3- container for liquefaction (refrigerator) of carbon dioxide gas. 44 3-3-4 High pressure pump
3-4- Conducting the hydraulic test of the device.
52
Chapter four: the method of conducting tests.
52
4 4-1- Materials used. .
53
4-2- Test method. .
54
4-3- Product analysis..
54
4-3-1- Scanning electron microscope analysis. .
55
4-3-2- image analysis software 3.2 (SIS). .
58
The fifth chapter: results.
58
5-1- Discussion and conclusion. 62 5-2- Effect of concentration. .
67
5-6- Conclusion.. .
69
Resources.. .
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