• 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:
    In mixing coal tar and/or coal tar pitch with aromatic and aliphatic solvents at atmospheric pressure and at a temperature between 15 DEG C and 140 DEG C to prepare a raw material for the manufacture of needle coke, the mixing ratio of the aromatic and aliphatic solvents and their quantities of addition to the coal tar and/or coal tar pitch are adjusted so that insoluble substances precipitate in a pitch zone. A supernatant obtained by separating the insoluble substances is distilled, and hydrocarbons consisting substantially of aromatic compounds and freed of the insoluble substances are obtained. Then the hydrocarbons are used as the raw material for the manufacture of needle coke.
    公开号:SU1052163A3
    申请号:SU772547452
    申请日:1977-11-25
    公开日:1983-10-30
    发明作者:Мигитака Ватару；Сунаго Хирофуми；Огава Юкиеси；Нисихата Таканори
    申请人:Ниттецу Кемикал Индастриал Ко,Лтд (Фирма)；
    IPC主号:
    专利说明:

    Mcphotic fattnfopumeftb i% Sec} na zvnshch, in a sheaf ujtow im gnawa snoln Aronatchey patMooptffneflb L (7 bes) On the jona. Kfncmff / i / ttf "eC to zone / Y Stc)
    2. A method according to claim 1, wherein the rout and so that the use of soft coal tar pitch with a softening point of 20-40 sec. Is used as coal tar pitch.
    3. The method according to claim 1 is also distinguished by the fact that a solvent selected from the group of creosol oil, flushing oil, anthracene oil is used as an aromatic solvent.
    4. The method according to claim 1, about tl and h am
    This is due to the fact that an aromatic solvent is used, starting points are boiling points of 140s and 60% by volume of components boiling up at 200-230 ° C, and 95% of components of boiling out components not boiling.
    5. The method according to claim 1 is also distinguished by the fact that a solvent from the group of gasoline, oil and kerosene is used as an aliphatic solvent.
    6. The method according to claim 1, about tl and h.a yu shch and with the fact that using an aliphatic solvent having an initial boiling point above and 95% by volume of components boiling off He above 250 ° C.
    7. The method according to claim 1, that is, and the fact that the ratio between the aliphatic solvent 1 and the aromatic solvent is 0.59: 1. :, .-. ; ;; . ; , ./ (.
    8. The method according to claim 1, of t. L. And h i and i with the fact that the ratio of the mixture between the solvent mixture "coal tar or pitch is 0.2-5: 1 .- ..:,,. :. ,; . ::, 9 The method according to p. 1, about tl and chakuyuschie and the fact that the processing conducts. At 70-140 C.: V:
    10. The method according to claim, 1 6 tons of l and 4ei y and y, so that merging in insoluble BeuiecTB is carried out by npV
    .20-100 C.:,,;,, :: ..,; . .,. ; ../
    11. Method: according to claim 1, about tl and h a "not with the fact that 1} is soluble
    substances are separated by gravity sedimentation and a pitch zone;
    The invention relates to the oil refining and petrochemical industries, in particular to methods for producing raw materials for the manufacture of needle coke by removing non-solvent substances containing quinoline-insoluble products from coal tar or coal tar pitch. A method for obtaining raw material for the manufacture of needle coke is known, which involves treating coal tar or pitch at temperature v - e - softening temperature of pitch with an aromatic solvent that boils above 120 ° C, and then separating insoluble substances by precipitating f1. However, it is difficult to remove insoluble substances from the coal tar clique using aromatic solvents having properties similar to those of the starting material. When processing a coal tar or pitch with a small amount of an aromatic solvent having a high dissolving cnoco-t property, the resulting mixture is too viscous, which does not allow for the effective separation of HepacTJBOpHMbDt substances. Insoluble substances can be precipitated and separated if the viscosity of the mixture decreases to a considerable degree with an increase in the amount of added carbon to the carbon. Noah resin or pek5 Aarsm «| Aticheskogo solvent. However, an increase in the amount of solvent added | g slightly increases the sedimentation rate of insoluble branches. The purpose of the invention is to accelerate the precipitation of insoluble substances and simplify the process. This goal is achieved in that according to the method of obtaining raw material for the manufacture of needle coke, including the processing of coal tar and and pitch ar1: (acid solvent and subsequent separation of insoluble substances by means of precipitates) to a coal tar or peck process an arsenic pattern. solvents at atmospheric pressure and a temperature of 15–140 ° C. As a coal tar pitch, use soft coal tar pitch having a softening point of 2040 ° C .; In addition, a solvent selected from the group of creosol oil, flushing oil, anthracene oil is used as an aromatic solvent. An aromatic solvent is used, having an initial boiling point above and 60% by volume of the components boiling away at 200-230 s, and 95 o6.% Of the components boiling away not higher. In addition, a solvent from the group of gasoline, not ti and kerosene is used as an aliphatic solvent. Moreover, an aliphatic solvent having an initial boiling point above and 95% by volume of components boiling away is not higher. In addition, the ratio between the aliphatic solvent and the aromatic solvent is 0.5-9: 1; the ratio between the mixture of solvents and coal tar or pex is 0.2-5: 1. The treatment is carried out at 70 ° C; separation of non-solvent substances is carried out at 20 -. Insoluble substances are separated by gravity precipitation in the pitch zone. . When processing stone tar pitch or coal tar pitch with bw of aromatic and aliphatic solvents, insoluble substances are precipitated in four zones, namely, in suspended, crystalline, pitch and oil, depending on the ratio in the mixture of the above three components. comnoHeHtoB., Insoluble substances can be precipitated either in the suspended, or in the crystalline, or in the pitch zone due to the regulation in the mixture of the ratio of the concentrations of the components: hard coal tar or coal tar pitch, aromatic and aliphatic solvent. Insoluble substances in the suspended zone are deposited under the action of gravity with an average speed of 1/10 - 10 mm / min, in the crystalline zone - 1/100 - 5 mm / m and in the pitch zone - at least 8 mm / m Insoluble substances , precipitating in the crystalline zone, are flat or flaky crystalline particles with a length of several millimeters; The substances precipitating in the suspension in the zone are particles of about 0.5-1. Substances precipitating in the pitch zone are resinous products, insoluble substances do not precipitate in the oil zone, but oily sludge may form. With appropriately regulated types and amounts of coal tar or coal tar pitch, aromatic and aliphatic diluents mixed with each other, the separation of insoluble substances present in the pitch zone can be accomplished not only by the mediocre use of such complex C1 as a pressure filter, and a centrifuge, but also through the use of such simple means as sedimentation by its own gravity and liquid cyclone. According to the method, the raw material used to make needle coke can be obtained on a scale. Insoluble substances in the pitch zone precipitate rapidly, and during their separation they can be easily carried out at a temperature of limited to 15 × without any increase in temperature. This provides significant advantages in the industrial implementation of the process. The starting material used in the proposed method is coal tar, which is formed as a by-product in the carbonization process of coal. The coal tar pitch used according to the method is a product that results in the fcIM polyamide, reducing the content of light oils in the coal tar as a result of distillation. Coal tar diluted with petroleum distillate mixed with light oils can also be used as a feedstock. Of these materials, the most preferred. is coal tar pitch, especially low-melting coal tar pitch with a softening temperature (determined by the ring and ball method) within 20–4 ° С and carbon residual, determined by Conrgshnson within 25–40 wt.%. The aromatic solvents used mainly consist of aromatic hydrocarbons and have initial boiling points of not lower and contain 95% by volume of components boiling up not higher. Most preferably, Nos. 1 are aromatic solvents which have an initial boiling point not lower than 140 ° C and contain vol.% By volume of components boiling away not higher. It is especially advisable to use solvents that have initial boiling points not lower and contain 60% by volume of components boiling between 200-230 ° C and 95% by volume of components boiling up not higher. KajiecTBe aromatic solvents use benzene, toluene, xylene, creosol oil, flushing oil, anthracene oil, oil formed during delayed coking, which is a byproduct of the process of producing raw pitch coke by the method of delayed coking, as well as their mixtures, distillation rates which are within the specified limits. The aliphatic solvents used consist mainly of al- ibic hydrocarbons, and have initial boiling points of not lower than 30 ° C and 90% by volume of components boiling higher. The aliphatic solvent was n-hexenzo-ligroin fraction, kerosene oil fraction, and gas oil. It is advisable to use aliphatic solvents that have starting boiling points not lower than 150 ° C and containing 95% by volume of components boiling up to not higher than 320 ° C. It is most preferable to use solvents that have initial boiling points of not lower and contain 95% by volume of components boiling up to not more than 250 s, for example, technical gasoline, gasoline-ligron fraction and kerosene fraction of oil. The method includes the steps of mixing these aromatic and aliphatic solvents with coal tar or with coal tar pitch at a temperature of 15, about the division of insoluble substances, distilling the supernatant obtained by removing insoluble substances. When mixing coal tar or coal tar pitch and. Of these two solvents, coal tar or coal tar pitch can be added first to the aromatic solvent at 15, preferably within 70-140 ° C, and then to the aliphatic solvent. In addition, the solvent can be simultaneously supplied to the coal tar or coal tar at the same time, in any case, the final precipitation of insoluble substances is usually the same. When adding solvents, the temperature is pre-set, the process is carried out at atmospheric pressure, the mixing time is 0.5 minutes and 5 hours. When using coal tar diluted with an oil distillate as a raw material, the quantities of solvents can be adjusted accordingly, Because this resin contains more aromatic oil than conventional coal tar. To achieve a uniform mixture of components and complete precipitation of insoluble substances, coal tar or coal tar pitch is mixed with solvents at 15-140 ° C, preferably 70-140 ° C. The drawing shows a composition diagram showing the precipitation of insoluble substances resulting from the treatment of coal tar or coal tar pitch with solvents (the amount of coal tar or coal tar, pitch and solvents affect the precipitation of insoluble substances), and the relationship between the ratio of mixture components is shown and the deposition of insoluble substances. Coal tar or stone peck and aromatic solvent mixed at a given temperature (point A). when an aliphatic solvent is introduced into the mixture at point B, planar forms or flocculent crystalline particles of insoluble matter begin to precipitate. Upon further introduction of the aliphatic solvent, the precipitated insoluble materials become viscous (point C). Black resinous substances are deposited on the bottom of the vessel (point t). Outside point D, the state of the insoluble substances remains unchanged, even if the introduction of the aliphatic solvent continues. When introducing an aromatic solvent into a mixture at point D, viscous flat forms, crystalline particles of insoluble matter begin to precipitate again at point E. When the aromatic solvent is further introduced, they turn into thin, flat forms of crystalline particles of insoluble matter a (point f). When replacing the aromatic solvent with aliphatic HepacTBOpHNuJte, the substances begin to turn into a grainy program at the point Q and turn into a fully Grained product at the point H and beyond. When replacing the injected solution | one on another, insoluble substances are deposited in different zones. The area between points A and B is defined as oil per zone, since in this zone oily substances are deposited. The region between points B and C, E is the crystalline zone, since flat crystalline substances precipitate in it. The region including the D point is defined as the pectonic eon, since black resinous substances precipitate in it. The region including the H point is the suspended zone, because suspended insoluble substances are deposited in this zone. The boundaries between the zones can be clearly defined by carefully observing the state of insoluble substances. Crystalline flat-shaped particles are non-porous, precipitated / precipitated, in crystalline form. zone reaches a length of several millimeters. Particles deposited in the suspended zone i have a diameter in the range of about 0.5–1 mm. In the pitch zone, viscous black resinous substances are deposited; they are deposited on the seabed and their softening points are usually higher than the softening points of the coal tar or coal tar pitch (measuring the softening points by the method, ring and ball). The ranges of individual zones in which insoluble substances precipitate in various forms depending on the ratio in the mixture of concentrations of coal tar or coal tar and two solvents vary according to the combination of solvents. In tab. Figure 1 shows the dependence of the change in the range of zones of deposition of insoluble substances during the processing of coal tar, depending on the combination of the solvent in the mixture and the ratio of the concentrations of the components of the mixture, wt.%: Table
    The points of the composition A, B, C, 6, E, F, G, H correspond to the points A, B, C, D, E, F, G, H on the diagram of cts1sta: va {cm, drawing).
    In tab. Figure 2 shows the dependence of the change in the range of zones of deposition of insoluble substances during the processing of coal | pitch depending on the combination of solvents in the mixture and the ratio of the concentrations of the components of the mixture, wt.%.
    Aliphatic
    Aromatic 50 solvent
    Naphthalene
    N-hexane oil
    Technical
    Naphthalene gasoline oil
    Naphthalene
    Kerosene oil
    Anthracene
    H-Hexane oil
    Technical
    Anthracene gasoline oil ITB a b l and c a The composition points A, B, C, D, E, F, G, H correspond to the points A, B, C, D, E, F, G, H on the composition chart (see drawing). Flushing oil (obtained by distilling coal) has the following characteristics: initial boiling point: 191 ° C; volume distillation at 60% 220С; 95% volume distillation. When (aromatic and aliphatic solvents such as benzene and hexane, respectively, are crystallized, the crystalline zone in the drawing is narrowed towards the center, while the suspended and pitch zones are expanded. Table 3 shows examples of mixtures used Solvents Table H Continued Table Aliphatic Aromatic Solvent Solvent Anthracene Kerosene Oil First Aid-Hexane Oil Technical Wash Gasoline Oil Wash Kerosene Oil Insoluble substances can precipitate various forms When entering into coal tar or coal tar pitch aromatic and aliphatic solvents in combinations / presented in T3 and adjusting the ratio of the concentrations of the components of the mixture, which is confirmed by the data presented in Tables 1 and 2. When choosing combinations of solvents and ratios of concentrations of solvents and at the same time ratios of concentrations of coal tar or coal tar can also precipitate substances in the suspension / crystalline or pitch zone. When treating coal from the coal pitch of the CBT using arsenic pitch solutions such as toluene, washing oil and anthracene oil, the insoluble substances obtained are transformed into very small particles and, of course, they are difficult to separate. When treating coal smb with aliphatic solvents such as n-hexane, yvrosii, and technical gasoline, precipitates of insoluble substances occur and they can be easily separated. However, in the surface layer, only low-molecular-weight layers were transferred, which comprised the components of coal tar and coal-tar Peck. Hydrocarbons produced by the race of the surface layer contain not a small amount of automatic ingredients of stone-like tar or coal tar pitch. When coking data with UHT1) a single coke yield, the low yield and the resulting coke do not have a well-manifested flow structure. Therefore, the use of one aliphatic solvents for processing does not provide a high yield of coke under industrial conditions of production from the obtained raw material. The use of a mixture of solvents for the treatment of coal tar or coal tar pitch. Provides easy separation of insoluble substances and leads to an increase in the yield of high-quality coke with a well-developed fluid structure during coking of the resulting raw material. Insoluble substances precipitate in the indicated zones at different rates. In the suspended zone, when they are deposited at an average speed in the range of 1/10 - 10 mm / mi, in the crystalline zone - 1/100 - 5 mm / min in the pitch zone with an average speed of at least 8 mm / min. The precipitates forming (cies in the pitch zone are viscous, black, and crumbly) collecting at the bottom of the vessel, and they are easily separated. Precipitated insoluble substances can be separated by precipitation under their own force of gravity, by means of a liquid cyclone, centrifuges and combinations of these means. The separation process does not require the use of high temperatures and can be carried out at 15 -, advantageously at 20. - It is advisable to use solvents that, regardless of their combination with each other, {from the floating layer after the separation process by distillation at atmospheric pressure or in vacuum. The solvents can be reused. In this distillation process, some lightweight buckets contained in the original coal tar or coal tar pitch are distilled In place of (| with solvent ks. The distillation process may be whose. Floated Layer that does not contain Insoluble Substances / is used as a raw material for the delayed coking unit. Paofritual can be regenerated & distillation column installation of the process of delayed coking. Example 1. One weight. including coal tar, containing 6f7 wt.% not soluble in toluene substances and 1.9 wt.% insoluble in quinoline substances, mixed with 1/2 weight.h. toluene and 1 weight.h. N-gvksana. The mixture is stirred at 80 ° C ohplajot up to 40c. Insoluble substances are precipitated and accumulate in the form of a black resinous product at the bottom of the vessel. After settling and separating the insoluble substances, the supernatant is distilled off under reduced pressure of 100 mm Hg. The product thus obtained has a softening point (according to the method of the ring and ball) and contains
    2.6% by weight of substances insoluble in toyuol and traces of substances insoluble in quinoline. As a result of coking the material obtained in an autoclave at a pressure of 2.5 kg / cm, crude coke is obtained with a well-developed fluid flow in 34% by weight. in the calculation of the original coal tar. Crude coke is baked and graphitized at 2900 ° C. The resulting product has a thermal expansion coefficient. -grad and the parameter Cpt6,7lS A (the length of the unit cell of the crystal lattice).
    P Rome p 2. -One weight.h. low-temperature coal tar pitch having a softening point of 23 ° C (determined by the ring and ball method) and containing 7.9 wt.% non-solutes in toluene of substances, is swept away and mixed with 1/6 weight, h. PRS 1by oil P1zi, and with 1/2 weight, h. technical gasoline 4. To 2201}. The mixture is cooled to. black insoluble smolisele sedimentation substance at a speed of 33 km / min. Insoluble substances
    they are separated by precipitation by their own force of gravity. The resulting evaporated layer is distilled off under reduced pressure of 100 km Hg. The product thus formed has a softening point (determined by the method 1 of the ring and the ball) and contains 5.2% by weight of toluene-insoluble substances and traces of substances insoluble in choline. As a result of coking under the conditions of example 1, crude coke with a well developed fluid structure is obtained with a yield; wt.% as calculated from the initial low-temperature pitch. Product,
    5 obtained after graphitization at 2800 s, has a coefficient of thermal expansion of 0.9x10 / deg and a parameter, 720 A, where C is the length of the crystalline unit cell
    0 gratings measured by X-ray diffraction.
    Thus, the proposed method makes it possible to obtain a raw material for the production of needle coke.
    权利要求:
    Claims (11)
    [1]
    1. A METHOD FOR PRODUCING A RAW MATERIAL FOR THE PRODUCTION OF NEEDLE COKE, comprising treating a coal tar or pitch with an aromatic solvent and then separating the Insoluble materials by precipitation, in order to accelerate the deposition of insoluble substances and simplify the process of grinding stone or a mixture of aromatic and aliphatic solvents at atmospheric Pressure and a temperature of 15140 ° С.
    A
    Aliphatic Solvent ('/ o Weight) May
    J Aromatic solvent (° / oats) Oil zone.
    Crystal zone o
    0 Coal sheaf a / or pitch pitch pitch 188 (tySec)
    [2]
    2. The method according to π. 1, characterized in that as a coal tar pitch use a soft coal tar pitch having a softening point of 20-40 ° C.
    [3]
    3. The method according to π. 1, characterized in that as an aromatic solvent, a solvent selected from the group of creosol oil, flushing oil, anthracene oil is used.
    [4]
    4. The method according to π. 1 of t n and w u h atm and with I d in that the aromatic solvent having an initial boiling point above 140 e C and 60 vol.% Comp boiling at 200-230 ° C, and 95 vol.% Of components boiling no higher than 300 ° C.
    [5]
    5. The method according to p. 1, characterized in that the solvent from the group of gasoline, oil and kerosene is used as an aliphatic solvent.
    [6]
    6. The method according to π. 1, characterized in that an aliphatic solvent is used having an initial boiling point above 150¾ and 95 vol.% Of the components boiling off no higher than 250 ° C.
    [7]
    7. The method according to π. 1, beginning with the fact that the ratio between the aliphatic solvent and the aromatic solvent is 0.59: 1. _
    [8]
    8. The method according to π. 1, about aphids and the fact that the ratio between the mixture of solvents and coal tar or pitch is 0.2-5: 1. '.
    [9]
    9. The method according to π. 1, with the fact that the treatment is carried out at 70-140 °. : l
    [10]
    10. The method according to π. 1, about l and yarn, and with the fact that the separation of insoluble substances is carried out pr * and 20-100'C.
    [11]
    11. Method: by π. 1, with the fact that insoluble substances are separated by gravitational deposition in the pitch zone;
    . 1 '
    类似技术:
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    US4582591A|1986-04-15|Process for the separation of resinous substances from coal-base heavy oils and use of the fraction obtained
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    同族专利:
    公开号 | 公开日
    PL202406A1|1978-07-17|
    DE2752511A1|1978-06-01|
    PL112247B1|1980-10-31|
    DE2752511C3|1980-08-28|
    JPS5366901A|1978-06-14|
    US4127472A|1978-11-28|
    JPS6041111B2|1985-09-13|
    DE2752511B2|1979-12-20|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US2871181A|1955-06-15|1959-01-27|Consolidation Coal Co|Method of removing finely divided solid particles from hydrocarbonaceous liquids|
    US2955079A|1956-11-26|1960-10-04|Texas Power & Light Company|Solvent extraction of low-temperature tar and products therefrom|
    US3147205A|1961-07-18|1964-09-01|Pittsburgh Chemical Company|Upgrading coal tar|
    US3617515A|1969-05-26|1971-11-02|Lummus Co|Production of needle coke from coal for pitch|
    US3799865A|1971-11-30|1974-03-26|Nittetsu Chem Ind Co|Process for producing needle-shaped coal pitch coke|DE2728605C2|1977-06-24|1986-03-27|Nippon Steel Chemical Co., Ltd., Tokio/Tokyo|Process for the production of acicular coal pitch coke|
    US4405439A|1979-07-25|1983-09-20|The Lummus Company|Removal of quinoline insolubles from coal derived fractions|
    DE2810332C2|1978-03-10|1982-08-05|Rütgerswerke AG, 6000 Frankfurt|Process for the separation of quinoline-insoluble constituents from coal tar pitch|
    US4277324A|1979-04-13|1981-07-07|Exxon Research & Engineering Co.|Treatment of pitches in carbon artifact manufacture|
    US4277325A|1979-04-13|1981-07-07|Exxon Research & Engineering Co.|Treatment of pitches in carbon artifact manufacture|
    DE3335316A1|1983-09-29|1985-04-11|Rütgerswerke AG, 6000 Frankfurt|METHOD FOR SEPARATING RESINY MATERIALS FROM CARBONATE HEAVY OILS AND USE OF THE FRACTION RECOVERED|
    DE3432886A1|1984-09-07|1986-03-20|Rütgerswerke AG, 6000 Frankfurt|METHOD FOR PRODUCING NEEDLE COOKS WITH LOW IRREVERSIBLE VOLUME EXPANSIONS FROM CHARCOAL TEE|
    JPH0321588B2|1984-10-05|1991-03-25|Kawasaki Seitetsu Kk|
    US4624775A|1984-10-22|1986-11-25|Union Carbide Corporation|Process for the production of premium coke from pyrolysis tar|
    DE3603883A1|1986-02-07|1987-08-13|Ruetgerswerke Ag|METHOD FOR PRODUCING CARBON TEERPECH RAW MATERIALS WITH IMPROVED PROPERTIES AND THE USE THEREOF|
    DE3609988C2|1986-03-25|1994-08-04|Metallgesellschaft Ag|Combined process for separating and treating asphaltenes with high softening temperature|
    DE3610375A1|1986-03-27|1987-10-01|Ruetgerswerke Ag|METHOD FOR PRODUCING A CARBON FIBER PRE-PRODUCT AND CARBON FIBERS MADE THEREOF|
    DE3636560A1|1986-10-28|1988-05-05|Ruetgerswerke Ag|METHOD FOR THE DESALINATION OF CARBON TARES AND PITCHES|
    DE3741482C2|1987-12-08|1990-10-18|Ruetgerswerke Ag, 6000 Frankfurt, De|
    US5534133A|1994-11-17|1996-07-09|Ucar Carbon Technology Corporation|Continuous method for increasing the Q. I. concentration of liquid tar while concurrently producing a Q. I. free tar|
    US5843298A|1996-09-27|1998-12-01|Ucar Carbon Technology Corporation|Method of production of solids-free coal tar pitch|
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    CN103421526B|2013-07-25|2014-08-13|张玮|Needle coke preparation method|
    CN105255510B|2015-10-12|2017-11-17|辽宁科技大学|A kind of method for determining that solvent method prepares refined bitumen technological parameter using phasor|
    US20170174999A1|2015-12-18|2017-06-22|National Chung Shan Institute Of Science And Technology|Method of manufacturing refined pitch|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    JP51141133A|JPS6041111B2|1976-11-26|1976-11-26|
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