• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
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    • 专利摘要:
    METHOD OF OBTAINING HIGH-CRYSTALLINE OIL COKE, including heat treatment and (raw petroleum feed at 430-520 C and pressure 4-20 kgf / cm for 30-500 s, rectification of heat-treated oil feed at 380-480 C and pressure 0-2 kgf / cm to remove impurities such as pitch or coke and to obtain purified heavy oil, heat the purified heavy oil to 450-550 ° C, unload it into the coking reactor and coking it at 450550 ° C and pressure 4-20 kgf per cm, characterized in that, in order to improve the quality of coke, purified heavy oil zhayut coking reactor downwards while injecting into the reactor On the inert gas from the bottom up and coking tempes paTypJy maintained by indirect heat exchange.
    公开号:SU1149880A3
    申请号:SU752175648
    申请日:1975-09-26
    公开日:1985-04-07
    发明作者:Хаяси Киесиге；Наканива Микио；Кобаяси Нобуюки；Ямамото Минору；Хасе Есихико
    申请人:Марузен Петрокемикал Ко,Лтд.(Фирма)；
    IPC主号:
    专利说明:

    .  ; 0 eo 11 The invention relates to the oil refining industry, in particular to methods. production of highly crystalline petroleum coke.  A known method for producing highly crystalline petroleum coke.  switch on (low heat sweet crude oil. up to 380-420 С and its subsequent coking at a given temperature and pressure of 2-10 kg / cm, separation of the obtained non-graphite coke from vapor-liquid products, fractionation of the latter into light fractions and heavy residue, heating of the heavy residue up to 400-460 С and subsequent delayed coking at 400–460 ° C and a pressure of 4–20 kg / sy 1.  However, this method is applicable only to crude oil as a starting material, but is not suitable for heavy bottoms obtained from the crude oil as a result of its rectification, cracking and other refining processes.  The closest to the invention is a method for producing highly crystalline petroleum coke, which includes heat treatment of the feed oil at 430-520 C and pressure of 4-20 kgf / cm for 30500 s, rectification of heat-treated.  oil at 380–48Cfc and a pressure of 0–2 kgf / cm to remove impurities such as pitch or coke and to produce very heavy oil, heat the purified heavy oil to 450,550 ° C, load it into the coking reactor, and then slow down coking it at 410-500 C and a pressure of 4-20 kgf / cm 2.  The method of delayed coking consists in that the initial oil feedstock, which is preheated to the temperature required for carrying out the coking process, is loaded into the bottom of the thermally insulated coking drum and held for a time sufficient to form coke.  In this method, the coking reaction, involving the processes of cracking, polymerization and condensation, is carried out under conditions of mixing the reaction mass with freshly loaded raw material Bbw material and light oil resulting from the cracking of the heavy oil during coking, as a result of which known difficulties are created in movement . growth and proper orientation of the formed coke crystals.  In addition, the quality of the coke formed varies depending on its position in the coking drum, as the fresh raw material passes from bottom to top through the coke already formed in the coking drum, and during this passage, the fresh raw materials to some extent undergoes coke, thanks to whereby the coke concentration becomes higher in the lower part of the drum, and correspondingly decreases in the part that is higher.  As a rule, coke produced at the bottom of the drum has a higher mechanical strength, but a worse value of the thermal expansion coefficient than coke produced in the higher located parts of the drum.  The main characteristic of the quality of Coke used in the electrode industry is e1; with the coefficient of thermal expansion (CTE).  In the electrode industry, coke with a low CTE is used.  In order to use coke in the electrode industry, coke of high quality with low CTE is sought.  The aim of the invention is to improve the quality of coke, reducing the coefficient of thermal expansion.  This goal is achieved by the fact that with the method of producing highly crystalline petroleum coke, including heat treatment of the initial petroleum feedstock at 430-520 s and a pressure of 4-20 kgf / cm for 30-500 s, rectification of the thermally treated crude at 380480 C and pressure 0 -2 kgf / cm to remove impurities such as pitch or coke, and to obtain purified heavy oil, heat the fine heavy oil to 450-550 ° C, load it into the coking reactor and coking it at 410-550 ° C and 4- 20 kgf / cm, purified heavy oil is loaded into the coke reactor neither from top to bottom while simultaneously injecting inert gas into the reactor from bottom to top and coking temperature is maintained by indirect heat exchange.  In assessing the quality of coke, it is advisable to determine not only KTR, but also the crush resistance of coke particles, the size of the crystals, the degree of their orientation.  The criterion for the quality of coke can be the magnitude of the maximum transverse magnetic resistance as an addition to the CTE value, or instead of it.  The higher the maximum transverse magnetic resistance, the better the size of the crystal formations, the degree of their orientation, and the packing density of the layers. e.  all the parameters that can decisively determine the quality of coke.  The maximum transverse magnetic resistance is determined by the formula f) H-po (fcp / p) T watc-p -tOO%, where p is the electrical resistance of the sample in the absence of a magnetic FIELD pI is the electrical resistance of the sample in a magnetic field.  The conditions for measuring these quantities are as follows: a magnetic field with an induction of 10 kgf, a temperature (liquid Ki and nitrogen) 77.  Said magnetic field is applied in the direction perpendicular to the sample.  f The magnitude of the maximum transverse magnetic resistance is highest in the case of a single crystal (single crystal) of graphite without defects, at a constant HdM magnetic field, decreases sharply with increasing degree of imperfection of the crystals and does not depend on the sample.  It has been established that the lower the CTE, the volume expansion coefficient (COR) and the electrical resistance, the higher the maximum transverse magnetic resistance, the coke crystal structure (texture) becomes more developed, the degree of orientation is improved, and the packing density of the layer increases.  Thus, since the magnitude of the maximum transverse magnetic resistance is in good agreement (well correlated) with the values of the CTE, COR and electrical resistance, as well as with the crystalline texture of coke, it is advisable to use this value as a reliable criterion for estimating quality coke for use in the manufacture of graphite electrodes.  The maximum coke transverse magnetic resistance is measured on a sample obtained by roasting raw coke at 1400 ° C for 3 hours, then grinding the burned coke into a powder to obtain fractions with a particle size of 35-65 and tOO mesh, further mixing for 40 hours.  fractions with a size of 35-65 mesh with 60 hours  fractions with a particle size of 100 n 30 hours  coal tar pitch, stirring and kneading the mixture during extrusion (extrusion on a screw press) of the kneaded mass in the form of a rod with a diameter of 20 mm and a length of 200 mm, sintering the molded mass at 1000 ° C for 3 hours and subsequent calcination at 2700 ° C for 1 h for the purpose of granitization.  The final stage of the process is the cutting of samples of a certain specific size and shape from the obtained graphite rod.  Petroleum coke, obtained in accordance with the proposed method, has a maximum transverse magnetic resistance of 16% when measured in the manner described and more than 50% when measured on graphitized coke obtained by graphitizing calcined coke at 2700 C within 1 hour  The petroleum coke produced by the proposed method has an unusual high-crystalline texture, has a characteristic silver-white metallic luster on the outside and is most suitable as a material for the manufacture of graphite electrons intended for use in ultra-high-power electric-arc furnaces.  First grade coke has a maximum transverse magnetic resistance of 6–10%, petroleum coke of the usual medium grade of a pelicina of maximum transverse magnetic resistance of 3–6%.  In tab.  1 shows the relationship between the magnitude of the maximum transverse magnetic resistance and the coefficient of linear thermal races in a direction parallel to the extrusion direction of the indicated types of petroleum coke, measured for samples made of artificial graphite, which in each case is obtained by the described method.  To produce high quality petroleum coke, t. e.  According to the existing quality scale, coke, which is considered to be first-class and highly suitable as a material for the production of high-quality graphite electrodes, the following conditions must be met: the starting material must have a minimum sulfur content; the content of light oil fractions in the starting material, as well as the amount of water vapor or inert steam supplied by blowing a bar into the coking bar to dilute the starting material, should be as low as possible (in order to limit excessive mixing of the reaction mass during the delayed coking reaction; the starting material should contain as low as possible and, even better, close to the trace amount of non-crystallized acid substances (t. e.  substances that are capable of forming, during coking, carbon of a noncrystalline structure), or contain such non-crystallized substances that can be almost completely removed by appropriate treatment.  The crude oil feedstock should have a low sulfur content. For direct distillation crude oil, the sulfur content should be in the order of 0.4 wt. % or lower, preferably 0.25 wt,% or less. .  For cracked fuel oil, the sulfur content should preferably be 0.8% or less.  The bottoms from the distillation of crude oil and cracked fuel oils containing a higher percentage of sulfur can be used, but only after they have undergone the desulfurization operation 80, 6 vania (desulfurization) in order to reduce the sulfur content in them to the required level.  As a raw material for the production of petroleum coke, it is also possible to use any other processed (refined) fuel oil, which is equivalent in its qualities to the specified substances.  FIG.  1 shows an installation diagram for implementing the proposed method; in fig.  2 - scheme of the coking reactor - coke crystallizer.  The installation contains a furnace 1 for preliminary. heating the raw material, pump 2 and pipeline 3 to feed the raw material to the furnace 1, the evaporative column 4, the pipeline 5 dJm to supply the raw material heated in the furnace 1 to the evaporation column 4, the pipeline 6 to drain pitch from the evaporation column 4, the pipeline 7 to drain vapor-gas products from the evaporation column, a heat exchanger 8 for cooling the vapor-gas products, a drum 9 for separating the uncondensed vapor-gas products from the condensed purified heavy oil, a distillation column 10, a pipeline 11 for feeding the non-condensing vapor-gas products from the drum 9 to the distillation column 10, the furnace 12 for heating the heavy oil to the coking temperature, the pipeline 13 for supplying the heavy oil from the drum 9 to the furnace 12, the coking oven 14 equipped with a housing 15 with a heating jacket 16, a nozzle 17 for supplying heavy oil to the coke crystallizer 14 located in the upper part of the housing 15, with a pipeline 18 located in the lower part of the housing for supplying a gaseous blow, with a pipeline 19 located in the upper part of the housing 15 to drain the gaseous pr ucts from the coking koksokristal. the pizator 14 to the distillation column 10, the hole 20 and the pipe 21 for unloading and discharging the resulting coke, the pipe 22 for supplying the heated heavy oil to the coke crystallizer 14, the heat exchanger-heater 23, the tank 24, the pipe 25 for feeding the heat carrier to the tank 24, the pipe 26 for supplying heat transfer medium from tank 24 to heat exchanger-heater 23, pipe 27 to feed heat carrier and heat exchanger preheater 23 to heating jacket 16 of coke crystallizer 14, pipe 28 for removing heat carrier from heating jacket 16, tank 2D, furnace 29, pipes 30 and 31 connecting furnace 29 with distillation column 10, pump 32 and pipeline 33 for supplying the bottoms from distillation column 10 to furnace 12, pipeline 3 for supplying fractions with a boiling point above 200 ° C to the suction inlet of the pump 2, heat exchanger. condenser 35, separator 36, pipeline 37, connecting distillation column 10 with heat exchanger condenser 35, pipeline 38, connecting separator 36 with distillation column 10, pipeline 39 for draining gaseous hydrocarbons from separator 36 and pipeline 40 for draining the liquid fraction from separator 36.  The installation works as follows.  The original oil tank is pumped out of storage by means of a pump 2 and is fed through conduit 3 to a furnace 1 intended for preheating.  In furnace 1, the crude feedstock is heated to an overpressure of 4–20 kg / cm and then kept at this temperature for 30,500 s in order to carry out partial cracking and thermal sinking of the feedstock.  Pre-heated crude oil feedstock is fed through conduit 5 to a high-temperature evaporation column 4, the upper plates of which are filled with special wire nets of addons designed to prevent the pitch from being carried along with the distillate in the process of intensive evaporation of the feedstock entering the column.  The pitch, having a softening temperature of 10-240 ° C, is discharged from the bottom of the column 4 through the drain pipe 6 in the molten state using an appropriate pump, while the temperature in the lower part of the column is maintained at 380-480 ° C at an overpressure of 2-10 kg / cm  Hydrocarbon fractions which, as a result of rapid evaporation at high temperature, passed into the vapor state, are removed from the upper part of column 4 through line 7 and, having passed through the cooling heat exchanger 8, enter the drum 9, where the condensed oil remains, anescondensed gaseous hydrocarbons are discharged via conduit 11 and is fed to the middle part of the distillation column 10.  The condensed heavy oil is pumped from the drum 9 through conduit 13 to the furnace 12, where it is heated to 450-550 ° C and fed further through conduit 22 to the upper part of the coking mold 14, where it is injected through the nozzle 17.  The heavy oil, heated to 450,550 ° C, is continuously supplied through conduit 22 through a valve to the upper part of the coke crystallizer 14, equipped with a heating jacket 16, where it is injected with the aid of a nozzle 17, while maintaining the temperature at 410,500 ° C and being under overpressure on the order of 4-20 kg / cm.  AT .  at the top of the coke crystallizer, there is an exhaust port through which a gaseous fraction of light hydrocarbons is led through line 19.  At the same time, the gummy fraction of heavy oil flows downwards and gradually accumulates there, undergoing at the same time transformations that make up the coking process.  The lower part of the mold is equipped with a pipe 18 through which a small amount of a gaseous mixture consisting of water vapor of a gaseous hydrocarbon and / or an inert gas, such as nitrogen, and heated to 400-500 ° C, is fed into the mold continuously. pipeline 18.  When the level of coke accumulated in the mold reaches the nozzle 17 or approaches. to it, the supply of heavy oil through conduit 22 is stopped and the amount of vapor-gas mixture heated to a high temperature and fed to the crystallizer through conduit 18 is sharply increased in order to ensure the removal of residual unbroken hydrocarbons from the crystallizer.  Upon completion of this operation of blowing residual hydrocarbons through the opening 20 and the pipe 21, the formed coke is unloaded from the coke crystallizer.  In order to maintain the temperature inside the coke crystallizer during the coking process at the level of 410-550 C, any suitable coolant, for example molten salt, superheated steam or a hydrocarbon stream heated to the appropriate temperature, in particular gaseous hydrocarbons withdrawn from the crystallizer, can be used. pipeline 19.  The heating jacket 16 is coated on the outside with an insulating material so as to minimize heat loss due to radiation.  Light gaseous hydrocarbons resulting from the evaporation of cracking and polycondensation of tar, similarly.  heavy oil, as well as a small amount of water vapor or gaseous hydrocarbons and / or inert gas, is removed from the coke crystallizer 14 through the exhaust hole located in its upper part, and through line 19 is fed to the distillation column 10, and the point of their entry into the column is located below the point of entry into the column of the pipeline 11.  In the outer heating jacket of the coke crystal of the lysers 14, the corresponding heat carrier is continuously circulating, thereby maintaining the temperature inside the coke crystallizers at the level of 410-500 C.  Circulation is carried out by supplying heat transfer fluid from line 25 through intermediate tank 24, through line 26, through heat exchanger YI heater 23, line 27 to pv6aiiiKy 16 of coke crystallizer 14, from which it is withdrawn via line 28 and returns to intermediate tank 24.  Salt melt can be used as a heat carrier.  To heat the coke crystallizer, light gaseous hydrocarbons discharged through pipeline 7 (temperature 450-550 C), pipeline 19 (gas mixture temperature 430-520 C) can be used as a heat carrier.  When the coke crystallizer 14 is filled with the formed coke, the supply of a heavy liquid to it is stopped and the stream of raw material is sent to another coke crystallizer, and at this time the fuel is discharged
    of coke from the coke crystallizer 14. Hydrocarbon fractions with so kip. higher than average
    for 260 seconds The feedstock is then introduced into the high-temperature evaporation column, supporting its tempering temperature 80 of the distillation column 10 in the form of a shoulder strap, taken directly from the column plates, and sent via conduit 30 to the furnace 29, where this distillation is heat treated under pressure at 500 -550 0, resulting in the formation of tar, and then returned via conduit 31 to distillation column 10, where it is introduced, along the height of the column, below the level at which the pipeline 30 is located. In the lower cube part of the column 10 there is an opening through which, with the aid of pump 32, a bottom residue is pumped out of the column and enriched with pegtem, which is pumped through conduit 33 to furnace 12, which is intended to heat the heavy oil along with the distillate. coming through the pipeline 13. Gas and gasoline fraction output from the upper part of the column 10, approach through the pipeline 37 through. heat exchanger-condenser 35 to separator 36, where gas is separated from liquid, the gas fraction is withdrawn through line 39, and the liquid fraction is divided into two parts, one of which is fed back to column 10 as reflux through column 38 The second is fed through pipe 40 to the finished product warehouse. In some cases, part of the distillate withdrawn from the tray of column 10 through conduit 30 can be connected via pipe 34 to the suction port of pump 2 to dilute the crude oil. received for processing, Example1. The cracking fuel oil containing 76% of sulfur, which is obtained as a by-product of conventional thermal cracking of gas oil (light diesel fuel), which is used to produce ethylene, and which has the properties given in table. 2, is used as a feedstock oil. The original SFE is introduced into a tube furnace having an inner diameter of 4 mm, an outer diameter of 6 mm and a length of 20 m, where it is heated to 490 ° C with an overpressure in the system of 4 kg / cm {{held at this temperature in AND 114 at 490 ° WITH. In the flash tower, the feedstock is rapidly evaporated to produce a distillate that is discharged through a pipeline at the top of the column. The pitch, formed in an amount of 20% by weight of the feedstock, is discharged from the bottom of the column after a certain period of time, equal to about 10 minutes. The gas generated in the process of raw material evaporation and pitch formation is removed from the column in the amount of 5% of the weight of the raw material introduced into the column. The heavy oil from the drum is passed through a tube furnace having an inner diameter of 4 mm, an outer diameter of 6 mm and a length of 4 m to heat up to 450 G, and then the heated oil is injected under a pressure of 9.0 kg / cm into the upper part of the coke crystallizer. In the coke crystallizer, there is a gradual accumulation and coking of the stack in the lower part of the tar-like heavy oil, the light, non-coking hydrocarbons are removed through the pipeline in the upper part of the crystallizer. The coke yield was 46.2%, based on the amount of raw material loaded into the coke-crystallizer (34.9%, based on the weight of the feedstock). In the process of cooking, 18.1% (13.6% calculated on the feedstock) of a cracked gas of 1.1% (0, g%) of gasoline with a boiling point are obtained. up to 200 28.9% (21.6%) gas oil with so kip. in the interval of 200-300C and 5.7% (4.3%) of heavy oil boiling above 300 C. The CTE (in the direction parallel to the direction of extrusion) in the temperature range of 100-400 ° Coke is 0.83 X 10 / C, and in the range of temperatures of software-ZOO. - 6.63 x maximum transverse magnetic resistance of 18% (all specified characteristics are measured for a sample of artificial graphite made from coke obtained in this example). Example 2. A hydrodesulfurized product is used as a feedstock, containing 0.3% sulfur, which is obtained from cracking fuel oil, containing 1.05% sulfur and obtained as a by-product in conventional thermal cracking of gas oil in an ethylene production system. The processing of this raw material is carried out in the same coke crystallizer in the same way and under the same conditions as in example 1. At the stage of rapid evaporation, pitch in the amount of 7.8% of the weight of the feedstock is withdrawn from the bottom part of the evaporation column. Gas was removed from the column in the amount of 0.8% by weight of the raw material. The output of coke is 22.8% calculated on the load of the coke crystallizer (i.e., 20% based on the weight of the feedstock). At the coking stage, 13.1% of the load of the coke crystallizer (12.0% by weight of the feedstock) of the cracking gas, 1.9% (1.7%) of the gasoline fraction with a boiling point are obtained. to 200 ° C, 53.2% (48.6%) of a fraction of light diesel fuel (gas oil) boiling at 200 ° C and 9.0% (8.2%) of heavy oil boiling above 300 ° C. Example 3. Gas oil (fraction boiling at 200-300 s), also called coke oil and obtained as a by-product at the stage of coking of example 2 (its properties are presented in Table 2), is introduced at a rate of 1 kg / h a furnace having an internal diameter of 4 mm, an outer diameter of 4 mm and a length of 40 m and subjected to thermal cracking at 530 ° C and a pressure of 65 kg / cm, a gel “string” (oil) boiling above is selected as thermal tar, and the unreacted the oil is recycled to the system to continue thermal cracking. 33.5% of the cracking gas, 29.9% of the gasoline fraction boiling in the range of temperatures up to, and 36.6% of thermal tar (calculated on the original gas oil), boiling up are obtained. The resulting thermal tar (heavy oil) is introduced into the coke crystallizer, which was used in Example 1, and coking is carried out under the same conditions as in Example 1. As a result, 47.3% of coke is obtained, 23.1% is cracked. gas and 29.6% cracking gas oil (calculated on the weight of thermal tar loaded into the coke crystallizer). EXAMPLE 4 The feedstock used in Example 1 was mixed with 0.5% (based on its weight) sodium hydroxide, taken as an aqueous solution. At the stage of high-temperature evaporation, the pitch in the amount of 29.0% is removed from the bottom of the evaporation column together with the gas fraction (1.1% by weight of the feedstock). After coking, a coke yield of 47.3% by weight of thermal tar loaded into the coke crystallizer (24.2% based on the weight of the initial sinter) in the process of coking (10.6%) gas cracking and 50.3% (35.1% ) cracking gas oil. Example 5. As a source of raw materials use the residue after the distillation of light fractions (hemispotron) from Minasovskoy crude oil, the properties of which are presented in table. 2. .. The specified feedstock is introduced into the furnace, the heating inner diameter 4 4 F1, outer diameter 6 mm and length 40 m, and heated under an overpressure of 20 kg / cm to 480 C and then kept at this temperature for 190 s . The raw materials subjected to heat treatment are introduced into a high-temperature evaporation column and subjected to rapid evaporation at atmospheric pressure and a temperature of 400 ° C in order to distill from it distillate discharged through the exhaust opening in the upper part of the column and remove the pitch that is extracted from the bottom of the column. (in the amount of 20.7% of the weight of the feedstock), after 15 minutes, during which it was in this bottom part, together with gas evolving in the amount of 21.0% of the weight of the feedstock. The resulting flash distillate (68.3% based on the weight of the feedstock) is passed through the furnace, heated to 450 ° C and injected under an overpressure of 9 kg / cm into the upper part of the coke crystallizer equipped with a heating jacket. During the process that takes place in the coke crystallizer, the tar-like heavy oil is progressively increased. it accumulates in the lower part of the apparatus and turns into coke, while the light unbroken hydrocarbons are removed through the exhaust hole in the upper part of the crystalline mash. Kok output, sa 5.9% based on the charge of the crystallizer (or 4.1% based on the weight of the feedstock). 80 At the coking stage, 18.2% (12.4%) of cracking gas, 20.0% (13.6%) of the gasoline fraction, distilled in the range t, kip, are obtained. to 200, 34.5% (23.6%) of the fraction of light diesel fuel (gas oil), distilled in the range of bp. –200300 С, and 21.4% (14.6%) of heavy oil boiling above 300 ° С. Example 6. Dzhatibarang oil of direct race, the properties of which are presented in Table 2, is used as the initial syf. 2. The specified feedstock is introduced into a furnace having an inner diameter of 4 mm, an outer diameter of 6 mm and a length of 40 m, and heated under an overpressure of 18 kg / cm to 480 s, maintained at this temperature for 300 s. After this heat treatment, the raw material is introduced into the drum, having a diameter of 100 mm and a height of tOOO mm, which is heated from the outside using an electric winding and coked at 415 ° C and a pressure of 3 kg / cm to remove non-crystallizing substances contained in the raw material coke. . The amount of coke formed at this stage, 1.0% from the web of the feedstock, is obtained 10.8% (based on the feedstock) of the cracking gas. The distillate obtained at this stage of coking (in the amount of 78.2% by weight of the raw material) is introduced into a furnace having an inner diameter of 4 mm, an outer diameter of 6 mm and a length of 4 m, is heated to 440 ° C (at the exit of the preheater) and then injected under an overpressure of 10 kg / cm into the upper zone of the coke crystallizer (similar to that used in Example 1), equipped with a heating head. The yield of the coke formed in the crystallizer is 11.2%, calculated on the crystallizer charge (or 8.8%, based on the weight of the feedstock). The properties of the coke obtained in Examples 1-6 are presented in Table. 3. Example 7. Illustrates the superiority of the technological system of coking, based on the use of the described coke crystallizer, over the system of delayed coking. For comparative experiments, the feedstock specified in Example 2 was used. In the first experiment, the raw materials, namely distillate from the high-temperature evaporation column, are preheated to 45.0 ° C in an oven that has an inner diameter of 4 mm, an outer diameter of 6 mm and a length of 4 m, and injected under an overpressure of 9 kg / cm into the upper zone of the crystallizer, used in example 1, equipped with an external heating jacket. In the second experiment, the same raw material is preheated by the same method as in the first experiment and then introduced into the conventional drum of the delayed coking and coked in the usual way. The results of the two experiments are presented in table. 4. Comparison of the results indicates a significant improvement in the properties of coke obtained in the first experiment {in accordance with the proposed method), compared with the properties of coke from the second experiment (obtained in accordance with the known method of delayed coking), in particular with respect to KTR, KOR and max. 194 transverse magnetic resistance. Example 8 (illostriruet advantages of the coking system according to the proposed method, based on the use of a coking crystallizer, as compared to the conventional system of slowed down. Coking in relation to the change in ketometry quality depending on its position on the height of the coke drum).
    Maximum transverse
    Coke magnetic resistance (10 kgf, 77 K),%
    Table 1
    The coefficient of linear thermal expansion (in excess of 100-400 ° C). For comparison, the two experiments described in Example 7 are reproduced using the same raw load. The properties of the coke obtained in these two experiments are determined in each case on several samples of coke taken in the upper, middle and lower parts of both drums for coking. The results are shown in Table. 5.. The results obtained indicate that a change in the quality of coke with a change in its position in the coke drum occurs to a lesser extent WHILE the coking process in the coke crystallizer (in accordance with the proposed method) than in the conventional delayed coking drum. For example, the CTE of coke obtained by the proposed method in the coke crystallizer, in the temperature range of 100-400 C, gives a dispersion (spread) of only 0.05-0.6 / whereas for coke produced in a conventional delayed coking drum, the dispersion em 0.110, 17x10 / s. The dispersion of the magnitude of the maximum transverse magnetic resistance for coke produced in the coke crystallizer is 0.1-0.4, whereas for coke produced in a conventional delayed coking drum, it is 1.3-2.2%. The coke produced by the method has an unusual highly crystalline texture and is superior in quality to petroleum coke of the highest grade.
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    with IO-ZOO C Maximum transverse magnetic resistance, Crush Crush resistance,, with COO-ZOO C 6.85 6.66 Maximum transverse magnetic 19.9 19.8 resistance,% Annealed Resistance times62, 7 73.8 pressure,%
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    权利要求:
    Claims (1)
    [1]
    METHOD FOR PRODUCING HIGH-CRYSTAL OIL COKE, including heat treatment of oil feed at 430-520 C and pressure 4-20 kgf / cm 2 for 30-500 s, rectification of heat-treated oil feed at 380-480 C and pressure 0-2 kgf / cm * to remove impurities such as pitch or coke, and obtaining purified heavy oil, heating the purified heavy oil to 450-550 ° C, loading it into a coking reactor and coking it at 450550 ° C and a pressure of 4-20 kgf / cm g , characterized the fact that, in order to improve the quality of coke, the purified heavy oil is loaded into a coking reactor from top to bottom while simultaneously injecting inert gas from the bottom up into the reactor, and the coking temperature is maintained by indirect heat exchange. _.
    SU <„> 1149880>
    1 1149880
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    SU1149880A3|1985-04-07|Method of producing high-crystalline petroleum coke
    US4100265A|1978-07-11|Process for preparation of high quality coke
    EP0374318A1|1990-06-27|Method for improving the properties of premium coke
    CA1154707A|1983-10-04|Coke production
    US7371317B2|2008-05-13|Process for producing coke
    RU2437915C1|2011-12-27|Procedure for production of coke additive by delayed coking
    US4551232A|1985-11-05|Process and facility for making coke suitable for metallurgical purposes
    US4199434A|1980-04-22|Feedstock treatment
    RU2560442C2|2015-08-20|Method for obtaining of coking additive by slow coking
    GB2083492A|1982-03-24|Production of pitch from petroleum fractions
    RU2085571C1|1997-07-27|Method of producing petroleum electrode pitch
    EP0455504B1|1995-03-29|Coking decanted oil and other heavy oils to produce a superior quality of needle-grade coke
    RU2058366C1|1996-04-20|Method for production of petroleum coke
    US4376015A|1983-03-08|Process for removing arsenic from green coke derived from shale oil
    US5071515A|1991-12-10|Method for improving the density and crush resistance of coke
    同族专利:
    公开号 | 公开日
    US4040946A|1977-08-09|
    JPS5144101A|1976-04-15|
    FR2286184A1|1976-04-23|
    GB1517975A|1978-07-19|
    DE2542842B2|1977-06-23|
    DE2542842A1|1976-04-15|
    JPS5431482B2|1979-10-08|
    FR2286184B1|1981-04-17|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    RU2537859C1|2013-06-18|2015-01-10|Государственное унитарное предприятие "Институт нефтехимпереработки Республики Башкортостан" |Procedure for oil residues thermal degradation|US2366057A|1941-02-18|1944-12-26|Standard Oil Dev Co|Process of coking hydrocarbon oil|
    US2775549A|1954-01-25|1956-12-25|Great Lakes Carbon Corp|Production of coke from petroleum hydrocarbons|
    US2921017A|1957-02-13|1960-01-12|Socony Mobil Oil Co Inc|Process of producing desulfurized coke from petroleum|
    DE1671304B2|1967-03-28|1976-05-13|DELAYED COOKING PROCESS FOR THE SIMULTANEOUS PRODUCTION OF TWO DIFFERENT GRADE OF PETROL COCKS|
    US3769200A|1971-12-06|1973-10-30|Union Oil Co|Method of producing high purity coke by delayed coking|
    US3736248A|1972-05-25|1973-05-29|G Hussong|Method for the manufacture of coke|
    JPS5431483A|1977-08-15|1979-03-08|Matsushita Electric Works Ltd|Manufacturing of pvc tile|US4927524A|1989-05-10|1990-05-22|Intevep, S.A.|Process for removing vanadium and sulphur during the coking of a hydrocarbon feed|
    US5891310A|1997-06-20|1999-04-06|Conoco Inc.|Delayed coking cycle time reduction|
    CN109052361A|2018-08-17|2018-12-21|东莞市凯金新能源科技股份有限公司|A kind of preparation method and soft carbon material of low cost soft carbon|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    JP10996674A|JPS5431482B2|1974-09-26|1974-09-26|
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