[Key words] Catalytic oil slurry; Heavy aromatics; Purification; Needle coke [Document code] A Catalytic oil slurry is a very special by-product produced during heavy oil FCC process because of its high density and relative molecular weight. Large, high viscosity and contain more fine-grained catalysts, limiting their use. At present, the catalytic oil slurry is widely used as a blending component of heavy fuel oil. It not only has low value of use, but also the fine powder of the catalyst will cause the nozzle of the furnace to wear, resulting in serious fouling of the surface of the furnace tube and a drop in thermal efficiency, affecting the furnace. Smooth operation, so the problem of catalytic oil slurry has been plaguing oil refining companies for many years. With the heavier quality of FCC processing raw materials, the output of catalytic oil slurry is getting bigger and bigger, and solving the problem of its outlet is particularly important.
Catalytic oil slurry contains a large number of 3 to 5 ring aromatic hydrocarbons with short side chains, which can be used as carbon black, needle coke, carbon fiber, rubber softener and filler oil, plastic plasticizers, road traffic asphalt and heat transfer oil. Such as high-quality raw materials for chemical products, but its solid content has strict requirements. Therefore, the precondition for the development and utilization of catalytic oil slurry is that the catalyst fines must be separated and removed to effectively reduce the ash content in order to meet the quality requirements of different applications. In recent years, a large number of researches have been conducted at home and abroad on catalytic oil slurry purification technologies such as sedimentation separation, filtration separation, electrostatic separation, and centrifugal separation.
This paper reviews the characteristics and research progress of sedimentation separation, filtration separation, electrostatic separation, centrifugal separation, and high temperature ceramic membrane cross-flow filtration, as well as the use of catalytic slurry in the chemical industry after purification.
1 Catalytic Oil Slurry Purification Technology 1.1 Sedimentation Sedimentation Sedimentation Separation consists of natural sedimentation and chemical sedimentation. The particle size of the catalyst fine powder in the catalytic oil slurry ranges from about 1 to 80 [mu]m, with particles of 20 [mu]m or less accounting for a considerable proportion. In the early stage of catalytic oil slurry purification, natural settlement separation method was used. The sedimentation process is usually carried out in a settler. The sedimentation speed of the catalyst fines in the settler is related to the size and density of the fines, the viscosity and the density of the slurry, and the like. Under certain temperature conditions, the larger the fine powder size, the faster the settling velocity. However, due to the fine dispersion of the catalytic oil slurry, on the one hand, the catalyst fines are very small, and on the other hand, the gums and asphaltenes contained in the oil slurry have the effect of hindering the sedimentation of the catalyst fines, so the separation and purification effect by gravity sedimentation is achieved. Poorer, generally needs to be clarified at a higher temperature of 250° C. and a longer time of 20 000 h, and the separation efficiency can reach 85. Moreover, it is difficult to remove the particles whose diameter is less than 20 μm by gravity, so the traditional natural settlement method has been Eliminating chemical sedimentation method is an economic and effective method developed in recent years. The addition of sedimentation agent can significantly increase the settling velocity and degree of removal of the fine powder of the catalyst. This method is not only easy to operate, but also has low investment [5]. Li Jinyun adopts the method of adding compound inorganic flocculants and organic flocculants, and the solid content in the catalytic oil slurry can be reduced to 0.65 mg/g after 80 h precipitation at 80° C., and the removal rate reaches 86.47. Niu Che et al. Demulsification flocculation sedimentation separation process, select PR3 compound as demulsifier dosage 100μg/g, Polyacrylamide as flocculant dosage 1 000μg/g, add pH=7, 30w glucose aqueous solution, settling temperature 90°C, time 12 h; Under this condition, the catalytic oil slurry ash content can be reduced to less than 100μg/g.
1.2 Filtration Separation Filtration Separation is the use of microporous materials to remove catalyst fines from the catalytic slurries. Changing the micropore diameter can achieve different filtration requirements. Precise filtration and separation can ensure that the quality of the filtered oil slurry after filtration meets the requirements of its deep processing. The key to filtration and separation is to select suitable filtering materials and effective backwashing methods. Catalytic slurry filter filter material is usually stainless steel powder or mesh porous metal sintered, filter pore size of 0.2 ~ 20μm. This filter has a high strength, can operate at high temperatures and can withstand high pressure. Since the 1980s, Mott and Pall in the United States have applied their respective filtration technologies to separate catalyst fines in catalytic oil slurries. The operating conditions of existing industrial plants are seen in the MPT high-efficiency pulse filter HyPulse LSI filter. For example, it is a tubular filter element filter, the filter element is LSS stainless steel powder sintered porous metal. Catalytic oil slurry flows from the bottom of the filter housing to the filter element. After the catalytic oil slurry passes through the filter element, it is purified and discharged from the upper part of the filter. The fine catalyst powder is intercepted and the filter cake is formed on the outer wall of the filter element. When the filter pressure drop occurs. After exceeding the allowable value, switch backwashing. The backwash uses a high pressure pulsed gas or liquid, passes through the filter element in reverse, and removes the cake. A standard HyPulse LSI filter system consists of three filters, one running online, one backwash, and one standby.
From the point of view of technical reliability and industrial applications, filtration technologies are used more often. Many domestic refineries have introduced filtration devices, but the filtering effect is not ideal. The mass fraction of catalyst fine powder in the catalytic slurry after filtration is 1 Above ×10, the system operation is complicated. When the filter is switched frequently for 1 to 2 h, it needs to be switched back flushing, and there are also problems such as easy blocking of the filter element, difficulty in cleaning and regeneration, frequent replacement of the filter element, high maintenance cost, and inability to operate stably. Some domestic oil refinery catalytic slurry filtration devices were abandoned because of poor results, and some were not put into operation after various reasons (911). It is difficult to meet the requirements of Cao Bingxi by using the filter separation method to treat the catalytic slurry. Catalytic Oil Slurry Purification Technology and Its Chemical Utilization Research Progress Petrochemicals Its Chemical Application Requirements.
1.3 Electrostatic Separation Method For the separation of catalytic oil slurry fines, U.S. Gulf Company developed the electrostatic separation method and realized industrialization in 1979. The separation principle is that when the catalyst slurry containing catalyst fines flows through a packed bed under the action of an electric field, the fine powder is polarized in the high-voltage electric field and adsorbed on the filler, so that the fine powder is separated. The separation efficiency is affected by the residence time of the material, the voltage of the electric field, and the physicochemical properties of the catalytic slurry. Under normal circumstances, as the voltage of the electric field increases, the separation efficiency increases, but when the voltage increases to a certain extent, the increase of the separation efficiency tends to be flat; the greater the viscosity of the catalytic oil slurry, the greater the deviation of the dielectric constant and the conductivity, and the separation efficiency. The lower. Catalytic slurry electrostatic separation suitable operating conditions: voltage 15 ~ 20 kV, residence time [12]. From the perspective of the operating conditions of foreign industrial installations, the main advantages of this technology are high separation efficiency, large amount of processing, low pressure drop, and easy flushing and regeneration. The disadvantages are large investment in equipment and high operating costs.
In 1988, Nanjing refinery introduced a set of US GA's patented technology and electrostatic separator equipment on the heavy oil FCC unit. The designed processing capacity is 10.5 t/h, and the catalyst fine powder content in the catalytic oil slurry can be from 1 g/L. Drop to 0.01 g/L or less. After several years of operation of the device, the separation efficiency is not stable enough. When the content of the catalyst fine powder is more than 6 g/L, the separation effect becomes worse.
Some domestic research institutes have conducted research on electrostatic slurry separation technology and equipment for catalytic slurries, explored separation mechanisms, and developed localized hardware. In 1994, they conducted industrial tests at Sinopec Zhenhai Refining & Chemicals Co., Ltd. However, since the effect of electrostatic separation is greatly affected by the change in properties of the catalytic oil slurry, and the experience of its use and operation is not fully understood, industrial applications are difficult. Therefore, the research and development of the electrostatic separation method is basically at a standstill in China 1.4 Centrifugal Separation Centrifugal Separation is a separation technique that uses centrifugal force obtained by the catalyst fine powder in the centrifuge much faster than its gravity to accelerate sedimentation to the wall. The catalytic slurry is heat-exchanged to a temperature of 150-300°C by a heat exchanger, and it is centrifuged at a high-temperature centrifugal separator. The centrifugation time is about 92-98. This method is a classical solid-liquid separation method and is simple and effective. However, the amount of catalytic oil slurry is too large and the operating cost is high, making it difficult to industrialize.
The hydrocyclone separation method is derived from the classical centrifugal separation method, and the key equipment used is the cyclone [16]. The principle of the hydrocyclone separation method is that the liquid-solid heterogeneous mixture is spirally moved in a cyclone at a relatively high flow rate, and the catalyst fine powder is separated from the liquid phase by centrifugal force. Theoretically, the cyclone can be separated from the fine powder size of 3 ~ 500μm, the fines in the feed can be as high as 30 mass fraction.
The cyclone has the advantages of simple structure, convenient operation, low equipment cost, small footprint, no rotating parts, and is widely used in many industrial fields.
The core of separation effect from the cyclone is the swirl field inside the device. After the material tangentially enters the separator, the spiral vortex rotates downward and the outer vortex spirals, and the inner vortex rises spirally from the cone bottom to the discharge port. The swirling field rotates. The power depends critically on the feed momentum. In order to obtain a good separation effect, sufficient feed and feed line speeds must be available. The results of the separation simulation test by Zhang Shirui et al. showed that the mass fraction of fine powder can be obtained after solid-liquid cyclone separation under the condition that the catalytic slurry feed flow rate is 3.5 L/min and the catalyst fine powder mass fraction is 5.2×10. To 1.8×10 4, the average particle size is 5.6 μm, and the removal rate reaches 96.5. If the hydrocyclone is used in series with two stages, the mass fraction of the fine powder after separation can be reduced to 5. It can be seen that the The effect of the flow device on the separation of the catalyst fine powder is very satisfactory, and it can meet the requirements of the catalytic oil slurry as the needle coke and carbon black raw material.
There are many factors that actually affect the cyclone separation process, including the structure of the cyclone: ​​the diameter of the cyclone, the size of the feed inlet, the diameter of the overflow orifice, etc.; there are process operations: feed pressure, flow rate, fine powder density And concentration, viscosity and density of liquid phase, and various factors affect each other, and if they are not properly designed or operated, the separation effect of the cyclone may be poor, and it is generally difficult to meet the final requirements for catalytic slurry filtration. Due to the simple structure and small footprint of the cyclone, it is sometimes used in practice as a pretreatment facility to reduce the load on downstream separation units such as filters. Sinopec Jiujiang Branch applied a cyclone pretreatment unit to the catalytic slurry filtration system.
1.5 High-temperature ceramic membrane cross-flow filtration method In 2008, Sinopec Changling Branch Co., Ltd. and Beijing Zhongtianyuan Environmental Engineering Co., Ltd. jointly developed a high temperature-resistant special ceramic membrane for the treatment of catalytic slurry filtration and its crossflow filtration processing technology. Cross-flow filtration: Under pressure, the raw material catalyzes the oil slurry to flow at a high speed on the surface of the membrane layer inside the membrane tube. The small molecular material liquid passes through the membrane in the direction perpendicular to the flow. The macromolecular material or the catalyst fine powder is retained by the membrane, making the fluid reach the Purpose of isolation and purification. In August 2010, a scale-up experiment of 500 kg/h was completed. The experimental results showed that the content of catalyst fine powder in the raw material catalytic slurry was 4.6 g/L, and the fine powder content of the catalyst after cross-flow filtration of high-temperature ceramic membrane was 0, The treated catalytic slurry can meet the technical requirements for chemical utilization. In December 2010, the technology passed the technical review of China Petroleum & Chemical Corporation.
Cao Bingyi. Catalytic Oil Slurry Purification Technology and Its Research Progress in Chemical Utilization The high-temperature ceramic membrane cross-flow filtration adopts a high-temperature-resistant ceramic membrane as a filtering material. This method not only has the characteristics of high filtration accuracy, but also overcomes the traditional The wire mesh filter needs frequent switching, easy plugging of the filter element and difficulty in cleaning and regeneration. Under normal circumstances, metal mesh filter method 1 ~ 2 h need to filter switching and backwashing, backwashing instantaneous pressure difference is large; and high temperature ceramic membrane crossflow filtration do not need backwash after dozens of hours of operation, and The backwash is gentle and no filter switching is required to achieve regeneration. The control system of the cross-flow filtration process of the high-temperature ceramic membrane is relatively simple, the requirements for the smooth operation are not high, and the industrialization is easy.
2 Catalytic oil slurries Catalytic slurries can be used to produce high value-added products such as carbon black, needle coke, rubber filling oils, plastic plasticizers, heat transfer oils and carbon fibers. Different products have different requirements for the content of catalyst fine powder in the catalytic oil slurry. For example, the production of needle coke requires that the mass fraction of fine powder is no more than 1×10 4; the production of carbon black requires that the fine powder has a small mass fraction 4. The production of carbon fiber requires fine The mass fraction of powders is not greater than in recent years. A lot of research has been conducted on the properties and rational utilization of catalytic slurries, mainly involving the combination of catalytic slurries and oil refining processes for the rational use of catalytic slurries, or on the composition of catalytic slurries. Study its use in the production of chemical products.
2.1 Needle-shaped coke needle coke is a high-quality variety vigorously developed in carbon materials in the 1970s. It is one of the artificial graphite, has a low coefficient of thermal expansion, low porosity, low sulfur, low ash, low metal content, high conductivity It is mainly used for the production of high-power HP and ultra-high-power UHP graphite electrodes and special carbon products for electric furnace steelmaking. It is also used for brush, battery and steel recarburizers, high-temperature high-quality refractory fillers. New Materials.
According to the coking mechanism of needle coke, the raw material for producing needle coke must have the characteristics of high aromatic content, excluding condensed-ring macromolecular aromatics, aromatic index BMCI of not less than 120, less impurities, and low content of ash metal, and during the thermal conversion process The medium has a higher mesophase transition temperature and a wider mesophase temperature range and can generate larger mesophase globules. Catalytic oil slurries are almost all aromatic hydrocarbons with short side chains and are the best materials for producing needle coke. In the mid-1980s, the raw material for needle coke produced in the United States was mainly catalytic slurry, and its production capacity was ranked first in the world. one. At present, there are only domestic needle coke production enterprises t/a of China Petroleum Jinzhou Petrochemical Company and t/a produced by Shanxi Hongte Coal Chemical Industry Co., Ltd. The products are basically used for HP graphite electrodes and cannot meet the production needs of UHP graphite electrodes. At present, the needle coke required for domestic UHP graphite electrodes mainly depends on imports. From the development trend of graphite electrodes, the development of UHP graphite electrodes is the mainstay, and ordinary electrodes will gradually exit the market.
In recent years, the import price and import volume of needle coke have increased year by year. The import price has increased from 10,888 yuan/t in 2007 to more than 16 000 yuan/t in 2010. In 2008, the import volume was. 4 kt. With the advancement of steelmaking industry technology and the increase of steel production, the demand for needle coke is increasing. At present, domestic demand for needle coke for graphite electrodes is about 2×10 t/a, but the domestic needle coke market is basically monopolized by imported products.
Carbon black is an important raw material for the production of rubber products and inks. The carbon black production requires that the relative density of raw materials is greater than 1.060, the kinematic viscosity residual carbon value is less than 10, and the mass fractions of sulfur, ash, asphaltenes, and water are high in the heavy aromatics content in the catalytic oil slurry and less impurities, and are used to prepare carbon black. High-quality raw materials, according to statistics, the world's 50 or more carbon black feedstock CBO is catalytic slurry, CBO ash content requirements for the 5 × 10 4, superior grade ash index is 3 × 10 or 4. Foreign use of FCC Light cycle oil and decant oil, as raw materials for carbon black production, have high yields, fine product particles and good strength, and are suitable as fillers for high-grade rubber products. In the metallurgical industry, they can be used as electrodes for advanced electric furnaces and can withstand strong thermal shock and Large current density. However, due to the high content of catalyst fine powder in the catalytic oil slurry, excess solids will accumulate in the heat treatment equipment and cause equipment corrosion, so the catalyst fine powder must be removed. In our country, it is urgent to develop carbon black production process using catalytic oil slurry as raw material.
2.3 Carbon fiber material Carbon fiber is a new type of material with high strength, high toughness, heat resistance, wear resistance, corrosion resistance, and radiation resistance. It is widely used in aerospace, military, medical, sports goods and other fields. Pitch-based carbon fibers have attracted much attention due to their high strength and high modulus characteristics and low prices. Catalytic slurry is a high-quality raw material for the preparation of carbon fiber, which can be used for the production of carbon fibers of medium and strong grades. However, it is necessary to remove the light components and catalyst fines in the catalytic oil slurry, and the solid content needs to be less than 10 μg/g. Currently, the countries with better development of asphalt-based carbon fibers are Japan and the United States. China is currently conducting pilot-scale R&D, and it is expected that industrial production facilities will be built in the next 2-3 years. Melt-blown low-melting mesophase pitch-based carbon staple fiber, high production efficiency, modulus up to 800 GPa or more, thermal conductivity is twice that of copper, is one of the basic varieties of carbon fiber petrochemical foam carbon is made of short carbon fiber and The charcoal/carbon composite made of resin carbon can be used as a filter element for filtration in high-temperature and strong-corrosion environments, and can also be used as a substrate for deep processing of carbon/carbon composite materials. At present, the prepared foamed carbon mainly uses mesophase pitch as a raw material, and the prepared foamed carbon can form a highly ordered graphitized structure, so it has good thermal insulation and electrical conductivity, and has the potential to become a new generation of functional materials and structural materials. Li Sizhong used carbon microspheres or toluene extraction to modify the mesophase pitch to obtain a foamed carbon with high compressive strength, and a carbon foam made from a mesophase pitch modified with 55w carbon microspheres. The compressive strength after 573 K is as high as 26.2 MPa, and the graphitization can still be maintained as 17.7 MPa after 2873 K. The foamed carbon prepared by the extraction of the mesophase pitch with toluene can achieve a compressive strength of 30 MPa after carbonization at 1573 K, and is graphitized by 2873. After K, it can still maintain 9 MPa; Lin Xiongchao adopts CAI process to modify the foamed carbon, and the apparent porosity before and after foamed carbon prepared at 400° C. and 5 MPa drops obviously, the reduction rate reaches 30, and the bulk density increases significantly. Large, from the first 0.434 catalytic oil-pore rich aromatic oil as raw material, after pyrolysis to prepare mesophase pitch, at atmospheric pressure to prepare a pitch-based 150-400μm pitch-based foam, and then in the muffle furnace carbonization to obtain a foam carbon. Cha Qingfang, etc. under the action of the catalyst p-toluene sulfonic acid, the catalytic oil-slurry-rich aromatic fraction and the cross-linking agent benzene dimethanol heated to 120 ° C or more to obtain an asphalt resin, the asphalt resin under certain conditions with carbon fiber or The carbon fiber paper was hot pressed to obtain a carbon / carbon composite.
With environmental protection increasingly attracting people's attention, carbon fiber will rapidly develop in applications such as aircraft, wind power, automobiles, and fuel cells. In 2010, China’s demand for carbon fiber also began to increase. It is expected that China’s carbon fiber demand will enter a period of rapid growth after 2012. 3 Conclusion Catalytic oil slurry is rich in heavy aromatics with short side chains, and is a valuable chemical raw material. Containing catalyst fines severely limits the application of deep processing. With the research and development of catalytic oil slurry purification technology, the application of catalytic oil slurry in chemical industry will increasingly attract more and more attention.
For catalytic oil slurry purification technology, on the one hand, we must do a good job in the research and development of new separation technologies, and on the other hand, we must do a good job in industrial conversion of new separation technologies. Therefore, it is recommended to cooperate with enterprises and research institutes to increase the removal rate of fine catalytic powders for catalysts for oil slurries; to step up the development of catalytic slurry chemical utilization technologies, especially for the production of needle coke, carbon black and carbon fiber materials from catalytic slurries. The technical study will strive to maximize the benefits of catalytic oil slurry utilization.
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