• 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:
    METHOD FOR CONVERSION OF COAL TO LIQUID PRODUCTS by preparing coal paste with a solvent consisting of a mixture of a fraction with a boiling point of 35-200 ° C and a recirculating residue after fractionation with a pour point of 20 ° C and having a beginning of boiling and an end of boiling, i-hydrogenating the paste in the presence of hydrogen and catalyst at 350-500 ° C, a pressure of 80300 atm and subsequent fractionation. The obtained liquid products, characterized in that, in order to improve the quality of fractions that are motor fuels, the initial coal is divided into two streams in a ratio of 3: 1-1t3, the first stream is mixed with the indicated solvent in a ratio of 1: 1.5- 1: 4, the second coal stream is mixed with a solvent having a boiling range of 200-DOO C and coal obtained by hydrogenation, in the same ratio followed by separate hydrogenation of both coal streams for 10120 minutes and then or by separate separation and fractionation of the products rogenization with the feed of the fraction of 35-200 ° C of the first stream as a solvent for the second stage of the coal stream, removing the fraction 35-200 of the second stream as the desired product, feeding the fraction 200-400C of the first stream and 16-100% of the fraction 200- 400 ° C of the second stream in g as a solvent for hydrogenation of the second coal stream, by withdrawing a possible excess of the fraction 200-400 0 as the desired product, feeding,. d tsasa of the residue above the first 400 ° C of the first and second streams to obtain a solution of the first hydrogenation stream of carbon "nei" and removal of excess in the form of the target product, or by simultaneous desalting and fractionation of hydrogenation products with a fraction of 35-200C as a solvent hydrogenerating hydrogenation of the first coal stream, feeding the fraction 200-400 ° C as the solvent for hydrogenating the second coal stream and feeding the residue above as the solvent for hydrogenating primary carbon noi with removal of excess fractions 35-200 ° C and 200-400S and possible excess BbMie residue as the desired product.
    公开号:SU1135430A3
    申请号:SU802935051
    申请日:1980-06-17
    公开日:1985-01-15
    发明作者:Ягер Беренд；Бринк Андрис；Клейнян Корнелис
    申请人:Сейзол Ван (Пти) Лимитед (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to the processing of coal, in particular to a method for converting coal to liquid products.  There is a known method for converting coal to liquid products by mixing carbon with a solvent, which is a mixture of thermally stable hydro-aromatic hydrocarbons at elevated pressure and temperature.  The resulting liquid products are separated from the solid phase and fractionated to obtain a gasoline fraction, fraction 204538 ° C, used for the production of motor fuels and a residue above 538 ° C.  Fraction 204-538 ° C. It is necessary to additionally subject to catalytic cracking to obtain motor fuels Cl.  The disadvantage of this method is the need for additional treatment of distillates, since they are not suitable as motor fuels without treatment.  The closest to the invention is a method for converting coal to liquid products by preparing coal paste with a solvent consisting of a mixture of a fraction with a boiling point of 35-200 ° C and a recycle residue after fractionation with a pour point and having a boiling point of 400 ° C. boiling at 600 ° C, taken in a weight ratio of 20-80; 80-20, hydrogenation of the paste in the presence of hydrogen and a catalyst at 350-500 ° C, a pressure of 80-300 atm, and subsequent fractionation of the products obtained from LI-1XX products 2 J.  The disadvantage of this method is that the engine fuel fractions must be pre-grilled before being used as fuel.  This additional treatment leads to a decrease in the final yield of high-quality fuel as a result of the formation of light fractions in the boiling range of gasoline.  But the quality of the light fractions should also be further improved by additional treatment, for example, by hydrogenation by cracking over a platinum catalyst so that they meet the requirements for carburetor fuel.  The purpose of the invention is to increase the fair fractions of motor fuels.  The goal is achieved by the fact that according to the method of converting coal to liquid products the initial coal is divided into two streams in the ratio 3: 1-1: 3, the first stream is mixed to form a paste with the specified solvent consisting of a mixture of a fraction with a boiling point of 35 -200Cj and recirculating residue after fractionation of the hydrogenation products of the first and second coal streams with a pour point of 20 ° C and having a boiling point of 400 ° C and a boiling end of 600 ° C in a ratio of 1: 1.5-1: 4, the second coal stream is mixed with a solvent having an interval boiling 200-400 ° C and coal obtained by hydrogenation, in the same ratio, followed by separate hydrogenation of both coal and catalyst streams at 350-500 ° C, a pressure of 80-300 atm for 10-120 minutes and then or separately de-ashing and fractionation hydrogenation products with the flow of fractions 35-200 ° C of the first coal stream as a solvent for hydrogenation of the first coal stream, removing fractions 35-200 0 of the second stream as the desired product, feeding the fraction 200-400 of the first stream and 16-100% of the 200- 400C of the second stream B as sol the hydrogenation agent of the second coal stream, removal of a possible excess of the fraction 200-400 C as the desired product, feeding the residue above 400 ° C of the first and second streams as a solvent for hydrogenating the first coal stream and withdrawing the excess as the desired product or the combined-i de-electrification) { by fractionation of the hydrogenation products with the supply of a fraction of 35-200 C as the hydrogenation solvent of the first coal stream, the flow of the 200-400 ° C fraction as the hydrogenation solvent of the second coal stream and the supply of the residue above 400 ° C The quality of the solvent for hydrogenation of the first coal stream with the removal of an excess of fractions of 35–200 ° C and 200–400 ° of possible excess of residue C in the form of target products and 2 is shown in FIG.  The technological scheme of the proposed method, the fraction with a boiling point of 35–200 ° C is hereinafter referred to as light, with a boiling point of 200–400 ° C, the residue after fractionation with a pour point of 20 ° C and the beginning of boiling of the AOO ° C and the end of boiling is a heavy fraction, the first stream (1), the second (11).  According to FIG.  1 source coal supplied by line 1, split two streams t and AND in a ratio of 3: 1-1: 3 Each stream is fed to successive stages of preparation of 2 coal pastes in an appropriate solvent, hydrogenation 3 pastes at ZZO-ZOO S and a pressure of 80-300 atm in the presence of hydrogen and a catalyst for the fractionation of 4 liquid products of the hydrogenation stage 3.  In addition, in the case of stream I, the hydrogenation products are subjected to preliminary separation into liquid and gaseous products and solids (ash and coke residue) J carried out at stage 5 of the ash removal.  At the stage of fractionation 4 of stream 1, a light fraction is obtained, which is fed as a solvent through line 6 to the stage 2 of preparing a paste, and the excess of the light fraction is withdrawn through line 7 as the desired product.  We then get to the fractionation stages 4 the middle fraction is withdrawn through line 8 and fed through line 9 to the stage 2 of preparing the paste from stream 11, and the excess of the middle fraction through line 10 is withdrawn as the desired product.  The residue after fractionation 4 through line 11 is recycled to cooking 2 paste coal stream 1, and the excess in the form of the target product is withdrawn through line 12 (it can be used, for example, for the production of electrode coke).  The by-products obtained at the stage of fractionation 4 of stream t (hydrogen sulfide, carbon dioxide and ammonia removed by washing, unreacted hydrogen that is recycled into the process, as well as carbon monoxide and hydrocarbon gases C. - The SD, which is subjected to reformed mngu to the hydrogen fed to the hydrogenation 3), is diverted along line 13.  The solids (coke residue, ash) are removed in stage 5 and withdrawn along line 14.  Here we are talking about solid substances of both streams 1 and 11.  At the stage of fractionation, 4 tt tats tatszhe receive a light fraction which in the form of the target product from 304 water through line 15, 16-100% of the middle fraction obtained at the fractionation stage 4 stream It The average fraction is fed through line 16 to the preparation of 2 pastes coal stream P, and a possible excess of the average fraction in the form of the desired product is diverted along line 17.  The residue after fractionation 4 of stream 11 through line 18 serves to prepare 2 pastes of coal and stream of t.  In the fractionation stage 4, the streams tl also produce by-products, which are withdrawn through line 19 and are processed or processed in the same way as the by-products of stream I, withdrawn through line 13.  According to FIG.  2 and :: the feed angle fed along line 1 is also divided by two. Flows I and II, each of which is treated and processed in the same way as the stream. chi 1 and c in fig.  one.  The embodiment of FIG.  2 is characterized in that the products of hydrogenation of both streams are subjected to a SOB localized clearing and frlciation.  The solids removed at the dezzola pani stage are discharged by HN) and 20.  The carbon contained in this residue is subjected to gasification and converted into iodine.  Essen. If one obtains a heavy residue, not containing coke and ash, the liquid product from stage 5 is fed via line 21 via distillation 22, where it is easily distilled off.  components that are fed to fractionated Hapocaiifse 4, and the heavy residue is withdrawn 23.  Head Nro. distillation distillate 22 is fed via line 24 to fractionation 4.  Products from stage 5 can also be mediocre. tpepu podgshlt on fraktsioinroBanis; by the value of 25, mine at this stage 22.  A part of the product 3 can be fed according to the latch 26 and 27 directly to the fractional 1P1e 4.  The heavy fraction obtained at stage 22 is usually measured as cf for the production of electrostatic coke.  IaiGyulye iiiiHro. :. uioJi for this YABL: er. The yellow fraction obtained from the hydrodynamic products of 3 streams I, the residue obtained during the processing of the drip C, is inferior in quality to the residue obtained from the processing of stream I, In this, the passage through stages 5 and 22 is mainly selected. from hydrogenation products 3 streams 1.  Moreover, almost the entire amount of hydrogenation products 3 stream 11 serves on line 27 directly to the fractionation 4.  As a result of the fractionation of hydrogenation products 3 supplied via lines 2A - 27 to stage 4, the following streams are obtained: stream 28, the middle fraction stream, which is fed as a solvent for hydrogenation of stream tl to the stage 2 of preparing the carbon paste; stream 29, a stream of light fraction, which is fed as a solvent for hydrogenation of stream t in step 2 of preparing a carbon paste; stream 30, a heavy fraction stream which, as the solvent for hydrogenation of stream 1, is fed to step 2 of preparing the carbon paste; stream 31, medium fraction stream discharged as the desired product; stream 32, light fraction, which in the form of the desired product is taken from fractionation stage 4j stream 33, a heavy fraction, which can be withdrawn as the desired product; stream 34, C, - hydrocarbon gases and other gases that can be processed into hydrogen, recycled to the process. Even if the heavy fraction is not withdrawn as the desired product, a certain amount of solids must be separated. stage 5 in order to prevent the build up of solids in the system.  In such a c-beam, the separation of solids should not be carried out very carefully. If the amount of heavy fraction obtained in stage 4 n is recycled through line 30, is; If insufficient, then the missing quantity can be replenished with a heavy fraction withdrawn from stage 22 and supplied through line 35.  Example 1  20P kg of washed coal with a grain size of "0.1 mm" is impregnated with a solution of molybdate ao-1 and then divided into two streams R of a 1: 1 ratio according to Fig. 1.  35 coal is used with the following composition,%: carbon 69.1, hydrogen 4.5j nitrogen 1.0 sulfur 0.4 oxygen 9, I ash 12.0 and another 3.2 when the content of volatile components is 37.6% After a day, both carbon streams contain 3.0 wt.% Molybdenum trioxide.  Both coal streams are fed to the paste preparation in the appropriate hydrogenation solvents.  At the same time, in both cases solvents and coal (including ash and moisture) are taken in a ratio of 3.0: 1. Both coal streams are subjected to hydrogenation at 450 ° C and pressure of 200 atm in the presence of hydrogen for 75 minutes.  The partial pressure of hydrogen is not critical inside the reactors and decreases from inlet to outlet of the reactor. In stream 1, the final partial pressure of hydrogen is usually lower than the pressure in stream tl. The following solvents are used to prepare coal paste: stream t stream P 32% light fraction 23% average fractions 200–400 ° C of 35–200 ° C from stream 1 of 1 54% heavy Lrac stream — 77% of the average (fraction 400–600) 200–400 ° C from stream 1 of tl 13% of heavy 400 BOOS fraction from stream L Further processing of both streams gives the following results.  As a result of the fractionation of stream 11, the following products are obtained: t4 kg of water, carbon dioxide and carbon monoxide, 11 kg of hydrocarbon gas Cj, 53 kg of light fraction, 36 kg of average fraction and 41 kg of residue.  In addition, another 3 kg of unreacted coal and 12 kg of ash are obtained.  The entire amount of residue is fed to the cooking pasta coal.  The total amount of the average fraction recycled from the fractionation stage to the preparation of paste coal stream 11,229 kg (86%). As a result of the fractionation of the products of stream J, the following products are obtained: 13 kg water carbon dioxide and carbon monoxide, 19 kg hydrocarbon gas C, 7 kg light fraction, 16 kg of residue and 71 kg of the middle fraction, which is recycled to the preparation of paste coal stream 11.  In addition, from stage 5, 7 kg of unreacted coal and 24 kg of ash are diverted.  From the stage of fractionation of the products of stream 1 to the preparation of the fifth coal of stream 1, a total of 100 kg of the light fraction and 159 kg of the heavy fraction are recycled.  Out of 200 kg of coal, only 27 kg of water, carbon monoxide and carbon dioxide, 30 kg of gas, kg of light fraction, 36 kg of medium fraction, 16 kg of heavy fraction, 7 coke, 24 kg of ash are obtained.  The coke residue is gasified to hydrogen.  In addition, hydrocarbon gases. and carbon monoxide is also converted to hydrogen by reforming.  The light fraction withdrawn as the desired product has an octane number of 91.6 and is characterized by the following quality: acidity 0.1 mg KOH / f; 0.01% sulfur; 15.4% pa Finnish hydrocarbons; 34.5% naphthenic hydrocarbons; 50.1% of aromatic hydrocarbons.  The average fraction from stream 1 having the cetane number 41 is diverted as the target product.  But the quality of this average fraction is inferior to the quality of the average fraction obtained in the form of the target product from stream 11, as evidenced by a comparison of data,%, according to the streams: Phenols 12.5 1.2.  PRI me R 2.  The example is repeated with the difference that the desired fraction is not withdrawn as the target product, but only the motor fuel. At the same time, 162 kg of coal 11 and 100 kg of coal are fed to the cooking of the paste of stream I.  The preparation of the coal pastes of both streams was carried out using the same circulating solvents in the same amount as in Example 1.  308 As a result of the processing of streams 1 and II, the following products are taken away from the system,% by weight of dry original coal, without taking into account ash: water, carbon monoxide and carbon dioxide: 13.2, gases C.  18.4, light fraction 28.5, average fraction 35.9, coke 4.1.  The resulting light and medium fractions have the same quality as in example 1 (the octane number is lightweight Fractions 91.7, and the cetane number of the average Lraction is 42-45).  PRI me R 3.  Use coal composition,%: carbon 56.6 - hydrogen 3.8; nitrogen 1,1; sulfur 2.9j oxygen 9.7; ash 23.1; And moisture 2.8 with the content of volatile components of 30.5%.  Example 2 is repeated with the difference that the process is carried out at a ratio of 1: 4 carbon and solvent.  The following products are removed from the system.  from the weight of dry original carbon, excluding ash, water carbon monoxide and doproxide uTlerod 12.1; gases C 17.2j light riipaKtsi 27.1; average fraction 34.6; coke 9.  The resulting light and medium fractions have the same quality as in example 1 (the octane number of the light fraction is 91.5, and the cetane number of the middle fraction is 42-45).  PRI me R 4.  Example 1 is repeated with the difference that the process is carried out at a 1: 1.5 ratio of carbon and solvent.  In this case, the following products,% of the dry raw coal pesa, are excluded from the system, excluding ash: water, carbon monoxide and carbon dioxide 13.5; gases 0.17.9; light fraction 27.6; average fraction 35.4; coke 5.6.  The resulting light and medium fractions have the same quality as in example 1 (the octane number of the light fraction is 91.8, and the cetane number of the middle fraction is A4-46).  PRI me R 5.  Example 1 is repeated with those listed in Table.  1 indicators and results.  The light fraction withdrawn as the desired product has the following characteristic: octane number 31.5 - 91.8; acidity P, 080, 1 mg KOI / g; 0,006 - 0,01% sulfur; 15.1 - 15.7% paraffin hydrocarbons 34.0 - 34.8% naphthenic hydrocarbons and 50.2 - 50.8% apochidic 9, hydrogen hydrocarbons, Ogodvn1-1 le in the form of uejieBoro p: products in the middle Fractions have clfi, p, yo shy characteristic; c tanoBoy number 41 - 46, 85.6 - 89 carbon 8.2 - 9.0% hydrogen 2.0% nitrogen; 0 „01 - 05.25% sGRA, 1.6 oxygen and 1 ,, O 13% phenol AND V and K 6, Repeat example with Choi, the difference is that recd1 - | 0 tidro z-chdii fovo, D); kt at j5 () C, Iri is from 20J kg UCP I get vpgo 28 bOAfj ,, oxy and carbon dioxide, 30 „3 kg gas C ,, - C ,,, 58 kg light fractional, 35 kg of the average fraction, 13 1G t of the fraction, kg. ok n 23 K jcjib Ji; :: iKaK rebrand and ke1 ok-oyucho number 9, 5 "a 1; to: anew what is cf (rac1t. AI 42, EXAMPLE 7 jTp-n-iept: isp.  Zuyut bovp coal SOS: Ta; 1 o / J: yrjLti 1od ЗЬ, hydrogen 4.1; ; erra 0.4; . , and the acid is 22.6, zs with the content. ne7y4; . srtP. iitiHHH waters (| ro; t; oi, atm:, e 120 f. riiH ,, Prp / LV ,. ) cat: Sora in the holistic my 1 from; K) H & Ug: and (rcsschn - cho as Pz (2 coal lioji;. i. p dusta: 60 hi odv. , school:, L: i. Gshua: / -1SI uG. SSSR.  / le odorod. ; s ra;;; Bj 75 kg lo: i O k; di; -lz 25 amidst ftk kipi, -. Rohr zagirov-gyshegs-, 10 kg yo php oti. T. ; rroBoe. gs pegk; V5; ii; p ;;; 9 I ,, 9, a d; t nCjBof of this BG1Doro /; n Irg, e-ro: asi LP to tJiHiJj 1 nairo 3010 Example 9 Repeat example 8 with the difference j that gdrogen: pressure 300 atm for 20 minutes  At the same time, the yield of the light fraction, having an octane number of 92, is oo; nIshayut up to 75 kg while reducing the yield of the average fraction to 5 kg, having a cetane number of 46.  I will try, AO. Repeat Hpfti iep 1 since | -; and 11, that the process is carried out in accordance with the flow chart of FIG.  2  At the same time, the source coal is divided into flows 1 and.  I in a ratio of 1s, 62: 1 and hydrogenation is carried out for 70 g-shn.  For the use of gases, which are immediately fed to fractionation 4, all product flows are fed to the cleaver stage 5.  Table 2 shows the composition of all the flows (coal total: 901.3 kg, in the deadwood state without sojiM, ash content: 125.8 kg, moisture drain. holding; 21.0 kg5 relative to noToicoB 1; it 1.62; one). .  B.  Experimentally, a lotter will be put in order to get 3 output fractions for the target product of the raw material, Ph05, EOA electrode coke, Iri-ucm source coal per riOTov: n i and il according to 1; 1 В r. -j. Djx, 3 y; -: aza1 (ssch; tav of all flowfiilBjO kg c.  iu: ar cocTciKuii angle, ash ash, content:. 6jO KG ;, moisture content: 16.0 kg.  soy: Goa:; tshi notation t i (p i m s p 1 i, Repeat pattern 10B with the difference ITO 282 kg (32. ) m. : The 1st fraction is discharged as a distant product. Octane numbers hp Gega dress: dii 9is2j and cetane -i.  average frakp l 43.  1 thus, the application of this application. Eolt t get light and medium fractions, KOTOp. ie sh- {okay octame and n. The ethane number, which) ia is better than the well-known method (; o6e.  iipi: h. 1st about GGAN number easy  yijbj a cetane number sredpsi Lrzchdni 45, fFTciiJonoa h. n layer light frakg1, ii 91. & , and the cetane number of an average gpakiiii 4),
    table 2
    (t stream)
    13.0 (tt flow)
    8.0
    26
    84.1
    120.5
    36
    44.3
    27
    55.9
    37
    20
    25
    28
    29
    1296.077.8
    1200,048.0
    458.6 1133.0101.9
    1060.4 263.060.6
    162.5
    1519.0 1296.0 1200.0
    648.0 Net 164, 8 262.8. One T he fraction is fully utilized in the genization of stream 1.
    (flow) 8.0 (flow 11) 8,, 0
    74.4
    26
    51.9
    36
    54,944,3
    27 37 20 25 21 23 24 28 29
    Table 3
    ADD, O 800, 6 1,200.0
    428.4 282.8699.6123.5
     1060,4163,060,6
    123.5
    90.1
    257.3
    637.0 62.6
    38.3 25.5 62.2
    38.3
    25.5 1200.0
    400.0 1296.0 319.0 O 162.5 as a solvent hydro 92, 74% by weight of the formation of a heavy fraction 7f26Z based on the weight of the heavy fraction.
    sixteen
    19 17
    Continued jra6Ji 3
    / Unreacted
    T wish
    coal + ash kg
     g
    eleven
    13 12
    11 7
    1rig.1
    权利要求:
    Claims (1)
    [1]
    METHOD OF COAL TRANSFER TO LIQUID PRODUCTS by preparing a coal paste with a solvent consisting of a mixture of fractions with a boiling limit of 35-200 ° C and a recycle residue after fractionation with a pour point of 20 ° C and having a boiling point of 400 ° C and a boiling end of 600 ° C, Hydrogenation of the paste in the presence of hydrogen and a catalyst at 350-500 ° C, a pressure of 80300 atm and subsequent fractionation of the obtained liquid products, characterized in that, in order to improve the quality of fractions that are motor fuels, the initial coal is divided into two the stream in a ratio of 3: 1-1: 3, the first stream is mixed with the specified solvent in a ratio of 1: 1.5-1: 4, the second stream of coal is mixed with a solvent having a boiling range of 200-400 ° C and obtained by coal hydrogenation, the same ratio, followed by separate hydrogenation of both coal streams for ΙΟΙ 20 min and then either separate desalination and fractionation of hydrogenation products with a fraction of 35-200 ° C of the first stream being supplied as a hydrogenation solvent for the first coal stream, removing the 35-200 ° C of the second flow in v e title product feed fraction 200-400 ° C and the first flow (6-100% fraction 200-400 C in the second stream as the solvent of the second coal hydrogenation stream diversion possible excess of 200-400 ° C fraction as the desired product, feed ,. residue above 400 ° C of the first and second streams to obtain a solvent of the first coal hydrogenation stream and removal of excess in the form of the target product, or by joint dehydration and fractionation of products of hydrogenation with a fraction of 35-200 ° C as a hydrogenation solvent for the first coal stream, by feeding fractions of 200-400 ° C as a hydrogenation solvent for the second coal stream and supply of a residue above 400 ° C as a hydrogenation solvent of the first coal stream with removal of excess fractions of 35-200 ° C and 200-400 ° C and possible excess and the residue above 400 ° C to form the desired products.
    with sl with se
    1,113
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    同族专利:
    公开号 | 公开日
    US4394215A|1983-07-19|
    BR8003775A|1981-01-13|
    DE3022581C2|1987-04-09|
    AU535387B2|1984-03-15|
    AU5934980A|1981-01-08|
    JPS564684A|1981-01-19|
    DE3022581A1|1981-01-29|
    GB2051855A|1981-01-21|
    PL127002B1|1983-09-30|
    US4318797A|1982-03-09|
    FR2459276A1|1981-01-09|
    FR2459276B1|1986-01-03|
    GB2051855B|1983-09-14|
    IN152877B|1984-04-21|
    ZW13380A1|1980-09-10|
    PL225055A1|1981-03-27|
    CA1171012A|1984-07-17|
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    申请号 | 申请日 | 专利标题
    ZA792997|1979-06-18|
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