• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    1518826 Petroleum coke MARUZEN PETROCHEMICAL CO Ltd 16 Sept 1975 [25 Sept 1974] 38065/75 Heading C5E A process for the production of coke from a petroleum feedstock such as crude oil or a residuum comprises the steps of preheating the feedstock 1 in a tube heater 2 to a temperature of 430-520‹C at a pressure of 4-20 Kg/cm<SP>2</SP>G for 30-500 secs; passing the preheated feedstock to a flashing column 3 where it is distilled at 380-480‹C, 0-2 Kg/cm<SP>2</SP>G to give a pitch which is removed from the bottom of the column at 6 and a distillate which is passed to a fractionating column 8; fractionating the distillate to give gas 21, gasoline 20, gas oil 17 and a heavy residue 10; and coking the residue 10 in drums 12, 13 by delayed coking at 430-460‹C, 4-20 Kg/cm<SP>2</SP>G for at least 20 hours. The coke thus obtained has a high degree of crystallinity and a graphite artefact thereof has a CTE (measured in the direction parallel to the extrusion) of less than 1.0 x 10<SP>-6</SP>/‹C over 100‹-400‹C. The pitch obtained from the flashing column may be coked by delayed coking at 410-430‹C, 2-10 Kg/cm<SP>2</SP>G to give a premium grade coke of low crystallinity. To improve the quality of the crystalline coke produced, alkali or alkaline earth metal salts may be added to the feed stock, sodium hydroxide and sodium carbonate being exemplified.
    公开号:SU999979A3
    申请号:SU752175498
    申请日:1975-09-25
    公开日:1983-02-23
    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:

    FIELD OF THE INVENTION The invention relates to the petrochemical industry, in particular, relates to a method for producing highly crystalline petroleum coke. The closest to the invention is a two-step method of delayed coking, which includes heating the feedstock oil to 380 - and then coking it at this temperature and pressure of 2-10 kg / cm, separating the resulting non-graphite coke from the vapor of fast-flowing products, fractionating the latter into light fractions and heavy residue, HeirpeB heavy residue to .400 - and its subsequent delayed coking at 400 and pressure of 4-20 kg / cm. However, the method is applicable only in those cases when using crude oil with a low sulfur content as a raw material and using a delayed type of coking as its first stage in order to separate non-crystalline substances from the raw material as non-graphitized coke so that to provide clean feedstock to produce highly crystalline coke. Such a delayed type of coking, used as the first stage, is quite expensive in its implementation and takes time. The main characteristic of the quality of coke used in the electrode industry is the coefficient of thermal expansion (CTE. In the electrode industry, coke with low CTE is used. In a known method, coke with CTE 0.98-10 is obtained at 100-400 C each. For using coke in the electrode industry is striving to produce high quality coke with low CTE. The aim of the invention is to streamline the process and improve the quality of coke - to reduce the CTE. This goal is achieved by the fact that of petroleum coke, including pre-heating of the crude to 430 — and a pressure of 4–20 kg / cm for 30,500 s, then it is subjected to a single evaporator before fractionation) at 380–48 (CW and O 2 kg / cm to remove pitch.
    In addition, the preheating of the crude oil is carried out in the presence of the basic compound in the forms of an alkali hydroxide or alkaline earth metal hydrate.
    At the same time, I take the main compound in the amount of 0.5 - 10 wt.% Based on crude oil.
    Moreover, oil raw materials are preliminarily heated up to 430-520С for 200-500 s.
    In the proposed method, a co-crystalline petroleum coke having a CTE in a direction parallel to the extrusion equal to or less than 1.0-10 at 100 - is obtained, the measurement is carried out on the sample as a graphite residue.
    Crude oil with a sulfur content of 0.4 wt.% Or below, a crude distillation residue, a cracking oil with a sulfur content of 0.8 wt.% Or below, and a sulfur-free product with a sulfur content of 0.8 &amp; % or lower, derived from any residue from distillation or cracking of petroleum.
    The drawing shows a diagram of one of the embodiments of the pre-laem process.
    Oil feedstock feeds the line.
    1c tubular preheater 2 without sludge with the addition of a small amount of hydroxide or carbonate of alkaline or alkaline earth metal that enters through line 3. In this preheater, the raw material is heated to a temperature of 430 — under a pressure of 4 to 20 kg / cm and maintained at this temperature 30 - 500 s, for which the cracking and swelling of raw materials. Heat-treated raw materials are sent to an evaporation column.
    4, where it undergoes a single evaporation. At the bottom of the evaporation column 4 coolant circulates through line 5 to maintain the temperature within 410 -. The heavy fraction of the thermally treated raw material with a temperature of 410-430c is discharged via line 6 through valve 7 as a resin. Distillate, separated from the resin in an evaporative column. not 4, is sent to the main fractionation column 8. In case the process conditions in the heater
    2stats so harsh that one-time processing of the raw materials in the evaporator column 4 is insufficient
    or blocking of the tubular preheater is inevitable, the preliminary heat treatment operation is modified as follows.
    A gas-liquid separator 9 is placed between the evaporating column 4 and the main column 8 to effect the condensation of a portion of the preheated raw material from which the resin is removed, and the condensate is recycled through line 10 to the preheater 2, where it is mixed with the raw material. Thus, a complete heat treatment is carried out in the preheater 2. The flash column 4 is equipped with a droplet separator 11 in order to avoid foreign and unwanted substances carried by the distillate entering the main column. The raw materials entering the main column 8 are mixed with it, with recirculated oil or thermal tar, and then discharged down the column through line 12 and sent to the coke heater 13. Heated up to 430 - the raw material is loaded through valve 14 into the drum 15 or 16 delayed coking, where it is subjected to coking at 430 - under a pressure of 4-20 kg / cm. The gas and light oil fractions, which are by-products in the coking drum, are discharged from the top of the drum through valve 17 and recycled to main column 8, where they are fractionated into gas, gasoline, gas oil and recirculating oil. Gas is removed from the top of column 8 through line 18, gasoline from line 19 and recirculated oil through line 12 and coking heater 13 after mixing with fresh raw material 1 at the bottom. Columns 8.
    The coking drums 15 and 16 are used alternately for delayed coking, they switch every 36 hours. While in one reaction there is a reaction, the coke formed is discharged from the other.
    The gas oil fraction produced in the coking drum through the main column 8 can be loaded via line 20 into thermal cracking apparatus 21, where it is subjected to thermal cracking at 510-550s under pressure of 35-65 kg / cm for gas, gasoline and thermal tar, which through line 22, they are recycled to the main column 8. Thermal tar is thus mixed at the bottom of the column with fresh raw materials and recycled oil, increasing the yield of coke. The gas oil fraction can be sent directly to distill the light fractions into the stripping column 23, where the light oil is removed, and the gas oil is withdrawn via line 24 and finds any desired application. In the latter case, the coke yield is lower, but the quality of the coke does not change.
    Example. As a raw material, thermal tar, called cubic tar, is used as a by-product.
    3 by the conventional thermal cracking process of gas oil in the production of ethylene with a sulfur content of 0.76% (its properties are listed in Table 1).
    Raw materials are sent to a stainless steel tubular heater with an inner diameter of 4 mm, an outer diameter of 6 &amp; mm and a length of 20 m with external heating using a heat transfer fluid, where it is heated under a pressure of 4 kg / cm to s is kept at this temperature for about 260 s. Then, the raw materials are sent to the middle part of the high-temperature evaporation column with a diameter of 100 mm and a height of 1000 mm with external heating using a wire electric heater. This column carries out a single evaporation of the raw material at 450 ° C under a pressure of 0 kg / cm and a retention time of 10 minutes at the bottom of the column, at the same time distillate is removed from the top of the column and the resin in the amount of 24.6% for raw materials in the amount of 5% for raw materials.
    The distillate is then sent to a fractionation column for separation. light fractions and heavy residue. The heavy residue is fed to a tubular heater with an inner and outer diameter of 4 mm and 6 mm, respectively, to be heated to the temperature required for subsequent coking, and is pressed into the coking drum, where it is subjected to delayed coking under a pressure of 9.0 kg / cm within 38 hours with a yield of 28.5% coke per charge (20% for raw materials). Coke by-products. neither%: gas 11.5 (3.1); gasoline with a boiling temperature of up to 25.4 415.2) / gas oil with a boiling point of JIOO-SrRH28.8.9 (17., 3, and heavy oil with a boiling point of 5.7 (3.4).
    1Trimer2. The raw material used is thermal tar, called ethylene-bottoms, which is obtained as a by-product in the process of conventional thermal cracking. Oil is used to produce ethylene with a sulfur content of 0.02%.
    A: The pipe is directed to a stainless steel tubular heater, the same as in example 1, is heated under pressure 4 and maintained at this temperature for about 260 seconds. The heated feedstock is sent to the middle part of the high-temperature evaporation column, the same as in example 1, where the Single Evaporation is carried out at and Okg / cm and the retention time is about 10 minutes with the release of distillate as head and resin from the bottom of the column in the amount of 17 , 7% for raw materials and gas in the amount of 2.6% per second.
    The distillate is sent to a fractionation column to be divided into light fractions and a heavy residue. A heavy residue is poured into a tubular heater, the same as in example 1, to be heated to the temperature required for subsequent coking, and loaded into a coking drum, where delayed coking is performed at 435 ° C under a pressure of 9.0 kg / cm for 38 hours, coke yield of 21.0% per charge (16.7% for raw materials). By-products of coking%: gas 7.3 5.8) / gasoline with a boiling point up to 200 ° C 25.1 (20, l) i gas oil with a boiling point 200-300 ° C 32.3 (25.7 and heavy oil with boiling point 300 ° C 14.3 (11.4).
    Approx. The raw material used is the residue of the distillation of light crude fractions.
    The raw materials are sent to a tubular nag, stainless steel revolver with an internal diameter of 4 mm, an external diameter of 6 mm and 40 m in length with external heating using a heat carrier, where it is heated under a pressure of 20 kg / cm to and maintained at this temperature is about 190 s. The thermally treated raw material is sent to the middle part of the high-temperature non-vaporizing column, where it is subjected to a single evaporation at 400 ° C and O kg / cm2 - and a dwell time of about 15 minutes at the bottom of the column, with the distillate being separated as the overhead and the resin as the lower overhead in the amount of 10 , 7% for raw materials, and gas in the amount of 21.0% for raw materials.
    The distillate is sent to a fractionation column for separation into light fractions and a heavy residue. A heavy residue is fed into the tubular heater, the same as in Example 1, to be heated to the temperature required for subsequent coking, and loaded into the coking drum, where the slowing down is carried out at a pressure of 9.0 kg / cm for 38 h, the output of coke to boot 5.9 (4.1% of the feedstock). By-products-coking%: gas- 18.2 (12.4); gasoline with a boiling point of 300 ° C 20.0 (14.6;.
    Example4. The procedures of Example 1 are repeated with some addition, the raw materials are mixed with an aqueous solution of sodium hydroxide in an amount of 0, 5% for raw materials. In the flash stage, a resin is obtained in an amount of 17.0% and a gas in an amount of 5.0%. At the stage of coking, poluchigoot coke with a yield of 34.5% on loading (26.9% on raw materials) and by-products,%: gas 15, 2 (AND, cracking fuel oil 50.3 (.39.3. Comparison of examples 1 and 4 shows the advantages are both in the output, fax and as coke, obtained by (the life of example 4. Example). The raw material is DJ atlbarang crude oil (its properties are listed in Table 1). The raw materials are sent to a tubular heater of stainless steel with internal 44 mm in diameter, b in outside diameter of b mm and 40 m in length with external heating by means of a heat carrier,: where it is heated under pressure (20 kg / cm before and kept at this temperature for about 230 s. Thermally processed raw materials, direct the middle part of a high-temperature evaporation column with a diameter of 100 with a height of 1000 mm and with external heating: with the help of a wire electric heater, where the raw material is evaporated at 400 s and O kg / cm and a retention time of about 5 minutes at the bottom of the column, with the distillate being separated as the overhead and resin as the lower overhead in the case of 12.0% feedstock and gas in the amount of 10.0% per feedstock. The distillate is sent to a fractionation column to be divided into light fractions and a heavy residue, the heavy residue is fed to a tubular heater with an inner diameter of 4 mm and an outer diameter of 66 mm for heating to the temperature required for subsequent coking, and loaded into a drum. coking, where slow coking is carried out at 9.0 kg / cm in 24 hours, coke yield 10.1% per feed (7.8%) on raw materials. Coking by-products,%: gas B, Q (7.6) i gasoline with a boiling point of up to 2 About 22.4 (17.5) - gas oil (37.5 and heavy oil with a boiling point of 300 ° C. 9.6 (7.5). Example. The raw material used is a desulphurized product containing 0.3% sulfur from cracked fuel oil, called desalted tar, which is obtained by desulphurisation of clous, which is a by-product of conventional thermal cracking gas oil in the production of ethylene (properties are given Table 1. Raw materials are sent to a stainless steel tubular heater with a diameter of 4 mm, external It is b mm in diameter, 30 m in length with external heating using a heat carrier, where it is heated under pressure of 20 kg / cm to 490 ° C and kept at this temperature for about 250 s. Then the raw material is directed to the middle part of the high-temperature evaporator column. 100 mm, 1000 m high and externally heated using a wire heater, where the raw material is evaporated once at 400 ° C and O kg / cm and a retention time of about 10 minutes for the column to separate the distillate as the overhead and the resin as the bottom chase, respectively in the amount of 7.9 for raw materials and 1.5% for raw materials. The distillate is then sent to fractionation column I for separation into light fractions and a heavy residue. The heavy residue is fed to a tubular preheater with an inner diameter of 4 mm and an outer diameter of 6 km to be heated to the temperature required for subsequent coking, and loaded into a coking drum, where it is carried out (delayed coking at 435 ° C and 9.0 kg / cm 2 in 38 hours, coke yield 10.9% per Boot, (9.9% in raw materials). By-products of coking,%: gas 8.6 (7.8) / gasoline with a boiling point up to 200 ° С 5.0 (5.5); gas oil 50/4 (45, heavy oil with a boiling point. 25.1 (22.11. Example 7). The procedure of Example 6 was repeated with some changes in g / n. Added to raw materials and 1% sodium carbonate in the form of an aqueous solution. The yield of coke is increased to 11.5% of the raw material and also improves its properties. The properties of the coke obtained in Examples 1-7 are given in Table 2. This coke belongs to the class of highly crystalline coke.
    权利要求:
    Claims (4)
    [1]
    Claim
    1. A method of producing highly crystalline petroleum coke from petroleum raw materials, including pre-cooked. efficient heating of the raw material, fractionation into light fractions and a heavy residue, heating of the heavy residue to 430 460 * 0 and its subsequent coking at 430 - 460 ° C and a pressure of 4 20 kg / cm g for 20 - 30 hours, characterized in that, in order to simplify the process and improve the quality of coke, the crude oil is preliminarily heated to 430 - 5 20® С and a pressure of 4 -20 kg / cm ^ * for 30 - 500 s, then it is subjected to a single evaporation at 380 - before fractionation 480 f C and a pressure of O -2, kg / cm ^ to remove the pitch.
    [2]
    2. The method according to p. 1, r and h βίο and with the fact that the preliminary 'heating of the crude oil is carried out in the presence of a basic compound in the form of an oxide of hydrate or carbonate.
    5 alkaline or alkaline earth metals.
    [3]
    3. The method of pop.2, characterized in that the main compound is taken in an amount of 0.5 - x
    10 10 wt.% Based on crude oil.
    [4]
    4. The method according to PP. 1 to 3, which is characterized in that the crude oil is preheated to 430-520 ° C for 200-500 s.
    fifteen *
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    同族专利:
    公开号 | 公开日
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    FR2286183A1|1976-04-23|
    FR2286183B1|1980-03-07|
    GB1518826A|1978-07-26|
    DE2542843A1|1976-04-15|
    US4049538A|1977-09-20|
    DE2542843C3|1978-07-06|
    JPS5144103A|1976-04-15|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    JP11031674A|JPS5431483B2|1974-09-25|1974-09-25|
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