WO1981000720A1 - Process for liquefying coal - Google Patents

Process for liquefying coal Download PDF

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Publication number
WO1981000720A1
WO1981000720A1 PCT/JP1979/000242 JP7900242W WO8100720A1 WO 1981000720 A1 WO1981000720 A1 WO 1981000720A1 JP 7900242 W JP7900242 W JP 7900242W WO 8100720 A1 WO8100720 A1 WO 8100720A1
Authority
WO
WIPO (PCT)
Prior art keywords
coal
aqueous solution
hydroxide
mesh
aqueous
Prior art date
Application number
PCT/JP1979/000242
Other languages
French (fr)
Japanese (ja)
Inventor
K Shimizu
Original Assignee
K Shimizu
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by K Shimizu filed Critical K Shimizu
Priority to GB8111221A priority Critical patent/GB2075046B/en
Priority to PCT/JP1979/000242 priority patent/WO1981000720A1/en
Priority to DE792953810A priority patent/DE2953810C1/en
Priority to DK106081A priority patent/DK161600B/en
Publication of WO1981000720A1 publication Critical patent/WO1981000720A1/en

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal

Definitions

  • the present invention relates to a method for liquefaction of coal without pressure, without heating and without hydrogenation.
  • the present inventor has proposed that granular coal already crushed in Japanese Patent Publication No. 54-155504 is immersed in an aqueous sodium hydroxide solution to form the granular coal. The solution is infiltrated and then the granular coal S: extracted?
  • the object of the present invention is at least one kind of
  • the coal liquefaction method of the present invention has a high temperature and high pressure ⁇ : It is not necessary, and it is simpler and more economical than the method described in Japanese Patent Publication No. 54-1155644.
  • the average particle size of the coal powder produced by a general pulverization method is 70 to 100 mesh, especially 100 to 200 mesh.
  • the aqueous hydroxide solution used in the present invention may be an alkali metal permanent oxide, for example, lithium hydroxide, sodium hydroxide, peroxidized lithium, or the like.
  • Trim ⁇ Aqueous solution containing sodium hydroxide and alkaline earth metal hydroxide produced during production, such as magnesium hydroxide, calcium hydroxide Aqueous solution or Jb hydroxide S: 2 types _S: Dissolved aqueous solution is applicable 3 Especially when manufacturing sodium hydroxide or sodium hydroxide by electrolytic method It is suitable to use by-product hydrated sodium-containing waste liquid and aqueous solution of hydroxylated lime.
  • coal powder may satisfactorily suspended and dispersed
  • the amount of the aqueous solution be at least 5 times, especially at least 2 times, the amount of the coal powder. powder rather by any method that can condition Sr maintained suspended dispersed in hydroxide aqueous solution, ⁇ , forced flow such as ultrasonic means favored arbitrary 3 these ⁇ in Pearl 5: Add You can do that too.
  • the suspending and dispersing time is, in principle, 1 hour until the oil component is generated as an upper layer, but generally 15 hours to 2 ⁇ s hours is sufficient. No further increase in Huai components is observed even after further disturbance S: after the oil components surface.
  • Solid layer Ru can and this Ru use as a liquefied raw material for at> its O or 0 ⁇ 3
  • Coal liquefied oil obtained in accordance with the present invention can be used as fuel as it is.
  • the three fractions, which distill from 150 to 1555 to 2444C, can be used as fuel. . Obtained by oil fractionation or rectification Each O component Petrochemical industry ⁇ Various corresponding
  • the process according to the present invention provides a method for
  • a petroleum smell is generated in the mixed system with a stirring time of 24 hours, and oily
  • Oil is dispersed and contained in the inside.
  • Example 1 Add 85 3 ⁇ 4 NaOH aqueous solution 45 o f ⁇ r to residual solid layer 200 f

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

A process for liquefying coal, which comprises stirring 70 - 300 mesh (on the average) coal dust in an aqueous solution containing at least one hydroxide of alkali metal or alkaline earth metal to suspend and disperse for a comparatively long time. The hydroxide aqueous solution preferably has a pH value of not less than 10.

Description

明 細 書  Specification
石 炭 の 液 化 法  Liquefaction of coal
技 術 分 野  Technical field
本発明は、 無加圧、 無加熱で且つ水素添加せずに 轻済的に石炭 §：液化する方法に関する  The present invention relates to a method for liquefaction of coal without pressure, without heating and without hydrogenation.
背 景 技 術  Background technology
従来、 石炭の液化法 と しては》 乾留法、 溶剤法等 が知 られているが、 とれ らはいずれも僅か ¾ エ ネ ル ギ一源 S:得る為に多大る エ ネ ル ギ ー δ:必要 とする と か、 高偭 ¾溶剤 §：必要 とする等の本質的 点 を 有 し てお ]? 、 工業的規模で実施 し得 も ©であつた。  Conventionally, as a coal liquefaction method, a dry distillation method, a solvent method, etc. are known, but all of them are only a little. Energy source S: a large amount of energy δ to obtain : Necessary or high temperature solvent §: It has essential points such as necessity etc.], and could be implemented on an industrial scale.
本発明者は、 既に特公昭 5 4 ― 1 5 5 0 4 号にて 铍砕 した粒状石炭 €：水黢化ナ ト リ ゥ ム水溶液中に浸 漬する こ と に よつて粒 石炭中に該溶液 滲透させ 次いで粒状石炭 S:取 ]? 出 し乾燥 した後に製粉機に て The present inventor has proposed that granular coal already crushed in Japanese Patent Publication No. 54-155504 is immersed in an aqueous sodium hydroxide solution to form the granular coal. The solution is infiltrated and then the granular coal S: extracted?
1 0 0 メ ッ シュ ¾下の粉末に し》 こ ©粉状石炭 S:水 酸化ナ ト リ ウ ム ぉ よ びカ ル ボ ン酸 S:含有した水溶液 中に入れ攪拌混合 し、 次いで石炭の液化が始ま る時 点ま で餑置 しそ して追加的る水 添加後に 9 0 〜 100 Mesh 粉末 Powder under the powder こ This powdered coal S: Sodium hydroxide び and carboxylate S: Put into the aqueous solution containing, stir and mix. Place until liquefaction begins and then add 90-
1 2 0 X： © —定温度に加熬する こ と Sr特徴 とする 、 石炭の液化法 ST提起 した 3 しか し更に研究 δ:重ねた 結果 以下 ©方法に よ って更に径済的に石炭 ©液化 ができ る こ X in した a  1 2 0 X: © — Coal liquefaction method with Sr characteristic of heating to a constant temperature, 3 proposed by ST, but further study δ: Overlapping results Below: Coal liquefaction by © method © Can be liquefied X in a
発 钥 © 開 示  Start 钥 © Disclose
即ち、 本発明対象は 、 少な く と も 1 種類のア ル力  That is, the object of the present invention is at least one kind of
OMPI OMPI
/ WIPO リ 金属 - ま たはア ル力 リ 土類金属水酸化物の水溶液 中に石炭粉末 §：攪乱させて比較的長時間懸濁分散さ せる石炭 ©液化法にあ る コ / WIPO Li Metal-or Al Li Coal powder in an aqueous solution of earth metal hydroxide §: Coal suspended and dispersed for a relatively long time by disturbing © Liquefaction method
本発钥 の石炭液化法は、 高温高圧 §：必要 とせず且 っ特公昭 5 4 一 1 5 5 6 4 号に記载 方法に比較 し て技街的に も 簡単であ ま た轻済的に も 有利であ 更には大規模に実旖する と と も 可能であ る - 発钥 S:実施する ための最良の形態  The coal liquefaction method of the present invention has a high temperature and high pressure §: It is not necessary, and it is simpler and more economical than the method described in Japanese Patent Publication No. 54-1155644. Advantageous and even possible to run on a large scale-invention S: best mode for implementation
本発明で使用される石炭は か ¾ る種類の も ので も よ く 、 例えば歴實炭、 褐炭、 亜炭お よ び無煙炭並 びに萆炭 > 泥炭等 ©未熟炭も 該当する 3 Since even the kind coal Ru ¾ or to be used in the present invention is also rather good, for example RekiMinorusumi, brown coal,萆炭to lignite your good beauty anthracite parallel Beauty> peat, etc. © immature charcoal also applicable 3
石炭粉末は一般的な粉砕手段に よっ て製造される 平均粒度 7 0 〜 S 0 0 メ ッ シュ 、 殊に 1 0 0 ~ 2 0 0 メ ッ シュ © も のが違 している 。  The average particle size of the coal powder produced by a general pulverization method is 70 to 100 mesh, especially 100 to 200 mesh.
本発明で用いる水酸化物水溶液は、 ア ル カ リ 金属 永酸化物、 例えば水酸化 リ チ ウ ム 、 水酸化ナ ト リ ウ ム 、 永酸化力 リ ゥ ム等 ©水溶液 電解法で水酸化ナ ト リ ゥ ム δ:製造する際に生する水酸化ナ ト リ ゥ ム含 有水溶液並びにア ル カ リ 土類金属水酸化物、 例えば 水酸化マ グ ネ シ ウ ム ， 水酸化カ ル シ ウ ム等の水溶液 ある は Jb記水酸化物 S: 2 種 _ S:溶解 した水溶液 が該当する 3 殊に水酸化ナ ト リ ゥ ム 、 電解法で水酸 化ナ ト リ ゥ ム 製造する際に副生する水羧化ナ ト リ ゥ ム含有廃液 よ び水酸化力 リ ゥ ム の水溶液が適し ている 。 石炭粉末と水酸化物水溶液 と ©混 合物 © ρΗ The aqueous hydroxide solution used in the present invention may be an alkali metal permanent oxide, for example, lithium hydroxide, sodium hydroxide, peroxidized lithium, or the like. Trim δ: Aqueous solution containing sodium hydroxide and alkaline earth metal hydroxide produced during production, such as magnesium hydroxide, calcium hydroxide Aqueous solution or Jb hydroxide S: 2 types _S: Dissolved aqueous solution is applicable 3 Especially when manufacturing sodium hydroxide or sodium hydroxide by electrolytic method It is suitable to use by-product hydrated sodium-containing waste liquid and aqueous solution of hydroxylated lime. © Mixture of coal powder and aqueous hydroxide solution © ρΗ
O PI O PI
A. WIPO - 値は p H 1 0 以上 殊に p H 1 1 〜 1 i 5 であ る のが好-ま し 3 石炭粉末 と水酸化物水溶液 と の割合 は、 石炭粉末が良好に懸濁分散 し得る程度であれば よ い - しか しなが ら 、 水溶液の量が石炭粉末に対 し て t 5 倍以上、 殊に 2 倍以上であ る と と が望ま しい 本発明 に於ける攪乱は、 石炭粉末が水酸化物水溶 液中に懸濁分散 した状態 Sr維持でき る方法であれば よ く 、 搜捽、 強制流動等が珠に好ま しい 3 これ ら © 楦乱に超音波手段 5:追加する こ と も で き る 。 A. WIPO - The value of Ru p H 1 0 or more particular p H 1 1 ~ 1 i 5 der virtuous - ratio between or Shi 3 coal powder and hydroxide aqueous solution, coal powder may satisfactorily suspended and dispersed However, it is preferable that the amount of the aqueous solution be at least 5 times, especially at least 2 times, the amount of the coal powder. powder rather by any method that can condition Sr maintained suspended dispersed in hydroxide aqueous solution,搜捽, forced flow such as ultrasonic means favored arbitrary 3 these ©楦乱in Pearl 5: Add You can do that too.
懸濁分散時間は、 原則 と して油成分が上層 と して 生 じる ま で ©時間であ るが、 一般に 1 5 時間〜 2 <s 時間で充分であ る 。 油成分が浮上 した後に更に攪乱 S:行なっ て も 淮成分の増加は認め られない。 油成分 O浮上後に撩乱 §:停止する 。 僅か 放置時間 の後、 混 合系は油性層 水性層 と 固侔層 （ ほ と んど未液化 石炭粉末 ） と の三層に分離する 3 油成層は殆んど油 であ ]) , 水性層中に も 相当量 O油が分散含 有されて いる - 石炭液化油は、 油性層お よ び水性層か ら 一投 的方法例えば蒸留に よ って得 られる 3 The suspending and dispersing time is, in principle, 1 hour until the oil component is generated as an upper layer, but generally 15 hours to 2 <s hours is sufficient. No further increase in Huai components is observed even after further disturbance S: after the oil components surface. Oil component O After ascending §: Stop. After a short standing time, the mixed system separates into three layers: an oily layer, an aqueous layer and a solid layer (almost unliquefied coal powder) .The three oil layers are almost oil.) significant amount O oil is distributed containing organic even during - coal liquefaction oil, 3 obtained I by the or al Itto methods such as distillation oily layer Contact good beauty aqueous layer
固体層は > そ Oま 0钦態で液化用原料 と して用 る こ と ができ る 3 Solid layer Ru can and this Ru use as a liquefied raw material for at> its O or 0钦態3
本発明に従って得 られる石炭液化油は そ © 5 0 上が 1 5 5 〜 2 4 4 C ま でに留出する 3 こ ©留 分は、 その ま 燃料 と して使用する こ と も で き る 。 こ の油 分留ま たは精留する こ と に よ っ て得 られる それぞれ O成分 石油化学工業 ©相応する種々 の Coal liquefied oil obtained in accordance with the present invention can be used as fuel as it is. The three fractions, which distill from 150 to 1555 to 2444C, can be used as fuel. . Obtained by oil fractionation or rectification Each O component Petrochemical industry © Various corresponding
分野で使用する こ と も でき る 。 It can also be used in fields.
本発明に従 う 方法は、 原油中の撺髡性の高 成分  The process according to the present invention provides a method for
€:増加させる Oに も 適用でき る - 本発明に従 う 方法 §: 、 実施例に よって更に詳細に  €: Applicable to increasing O-method according to the invention §:, further details by example
説明する 。 但し本癸明はか ^ る実施例に限定される explain . However, the present invention is limited to this embodiment.
も Oではない。  Nor O.
実施例 1 Example 1
1 0 0 メ ッ シュ の歴實炭粉末 （ 太平洋炭 ） S 0 0  100 Mesh's actual coal powder (Pacific coal) S 0 0
f §: 3 ビー カ に仕込み、 Cl 8 5 iiaOE 水溶液  f §: Charged into 3 beakers, Cl 8 5 iiaOE aqueous solution
6 5 0 9 §：添加する 。 こ O混 合液の出発時 pH- 値は  6 509: Add. The starting pH-value of this O mixture is
約 1 2 であ る 3 こ ©混合液に 、 長さ 羽椟 §： About 1 2 to 3 this © mixture Ru der length Hane椟§:
有 した授拌手段に て 5 0 0 〜 る 0 0 回転ノ分 授拌 Hand 5 0 0 Ru - in a closed-the授拌means 0 0 rotation Roh minute授拌
行な う 3  Do 3
2 4 時間 の攪拌時間で混合系に石油臭が生 じ油性  A petroleum smell is generated in the mixed system with a stirring time of 24 hours, and oily
層が生ずる 3 攪拌停止後油性層 の下に生ずる水性層 Layer formed 3 Aqueous layer formed under oily layer after stopping stirring
中に も 油が分散含有されている為》 油性層 と 共に水 Oil is dispersed and contained in the inside.
性層 も 一緒に蒸留処理に委ねる 3 蒸留 ©結果、 涕点 3 distillation that also submits to the distillation process together with the functional layer.
1 5 0 C 以上 2 4 4 X： 以下 ©油成分 ό 2 ί1並ひにそ 1 5 0 C or more 2 4 4 X: or less © Oil component ό 2 ί 1 line
れ以上の漭点 Ο油成分 5 1 f が得 られた 。 An oil component of 51 f was obtained.
実施例 2 Example 2
α 8 5 ¾ Na OH 水溶液の代 ]? に * 電解法で Na OE  α 85 ¾ instead of NaOH aqueous solution]?
製造する際に副生する Na OH 含 有量 4 5 廃液  NaOH content by-product during manufacturing 4 5 Waste liquid
§：水に加え て造った α 6 5 * Na OH 水溶液を用いそ §: Using α65 * NaOH aqueous solution made in addition to water
して混合液 ©出発時 pE- 値が約 1 2· 8 であった泡は Mixture © Foam with pE- value of about 12.8 at the start
Ο ΡΓ _ 、 ,， V IFO ¾ ノ 実施例 1 §：繰返 した ： > Ο ΡΓ _, ,, V IFO ¾ Roh Example 1 §: repeated:>
と 場台には、 涕点 1 5 0 € ^ _b 2 4 以下 O 油成分 6 4 f 並びにそれ _fc ©裨点の油成分 4 9 f が得 られ ft ,  On the ground, the point is 1550 € ^ _b 24 or less O oil component 6 4 f and its _fc © oil component 49 f are obtained ft,
実施例 5  Example 5
α 8 5 * NaOH 永溶液の代 ！） に、 α 8 4 * ΟΗ 水 溶液 s 0 Ψ を用いそ して混 台液 ©出発時 ΡΕ 値が 約 1 & 5 であ る池は、 実 ¾例 1 繰返した 。 α85 * NaOH Eternal solution fee! To), α 8 4 * and ΟΗ water solution s 0 Resona using the Ψ mixed base solution © starting when Ρ Ε value is about 1 & 5 Der Ru pond, was repeated real ¾ Example 1.
こ の場台には、 漭点 1 5 0 で 以上 下の 油成分 5 8 f 並びにそれ _h ©涕点の油成分 4 9 f が得られ ft  At this point, the oil component 58 f at the 漭 point 150 and the oil component 49 f at the _h ©
実施例 4 Example 4
実施例 1 ©残留固佯層 2 0 0 f に 8 5 ¾ NaOH 水溶液 4 5 o f §r添加する - こ の混台液 O出発時  Example 1 © Add 85 ¾ NaOH aqueous solution 45 o f §r to residual solid layer 200 f
ΡΗ 値は 1 3· 6 であった 3 の処理は実施例 1 に記 載の如 く 行 ¾ う 3 ΡΗ value 1 3.6 a a three process embodiments如rather row ¾ Cormorants 3 mounting serial 1
と の場台には、 沸点 1 5 以上 2 4 4 C 以下の 油成分 4 0 f 並びにそれ以上 O粽点の油成分 S 1 9 が得 られ ft。  At the bases of and, an oil component with a boiling point of 15 or more and 24.4 C or less and 40 f or more, and an oil component of Ozumi point S 19 were obtained ft.
産業上の利用可能性  Industrial applicability
本発明に従って得 られる石炭液化油は ¾ そ © 5 0 も 以 が 1 5 5 〜 2 4 4 1C ま でに留出 し、 か る留 出成分はそのま ^燃料 と して使甩する こ と がで き る 。 ま たと の油 を分留ま たは精留する こ と に よ っ て得ら れるそれぞれの成分 、 石油化学工業の相応する種 Component output coal liquefied oil obtained distillate ¾ its © 5 0 even than is distilled to 1 5 5 ~ 2 4 4 1C until in, that if in accordance with the present invention and this is甩used as its or ^ Fuel I can do it. Each component obtained by fractionating or rectifying other oils, the corresponding species of the petrochemical industry
OMPI
Figure imgf000008_0001
OMPI
Figure imgf000008_0001
Θ Θ

Claims

請 求 の 範 囲  The scope of the claims
(1； 少 ¾ く と も 1 種類 の ア ル カ リ 金属 - ま た は ア ル  (1; at least one kind of Alkali metal-or Al
力 リ 土類金属水酸化物 ©水溶液中 に石炭粉末 §：攪 乱させ て比較的長 時間懸濁分散させる 石炭 ©液 化法 s Power Earth-metal hydroxide © Coal powder in aqueous solution §: Suspended and dispersed for a relatively long time by dispersing coal © Liquefaction method s
(2) 水酸化物水溶液が NaOH- ま た は KOH 水溶液ま た  (2) The aqueous hydroxide solution is NaOH- or KOH aqueous solution or
は電解法 で liaOH S:製造する 際 に生ず る N a OH 含 有廃液で あ る特許請求の範囲第（1)項記載 の方法：》  Is liaOH S by the electrolytic method, which is NaOH-containing waste liquid produced during production. The method according to claim (1): >>
(3) 石炭粉末の平均粒度が 7 0 〜 3 0 0 メ ッ シ ュ 、  (3) The average particle size of the coal powder is 70 to 300 mesh,
殊に 1 0 0 〜 2 0 0 メ ッ シ ュであ る特許請求の範 囲第（1)項 ま たは第（2)項記載 の方法 - In particular, the method according to claim (1) or (2), which is a claim of 100 to 200 mesh-
(4) 水酸化物水溶液 の pH- 値が 1 0 以上で あ る 特許 (4) Patent in which the pH value of the aqueous hydroxide solution is 10 or more
請求の範囲第（1)〜（3)項 Οいずれか一つ に記載 の方 czi The method according to any one of claims (1) to ( 3 ).
(5) 撩乱 ¾： 撹拌に よ っ て行な う 特許請求の範囲第（1)  (5) 撩 ¾: Claims (1) to be performed by stirring
〜（4)項の ずれか 一つに記载 方法 3 ~ (4) Ki载method 3 Zureka one term
O PI _ O PI _
PCT/JP1979/000242 1979-09-11 1979-09-11 Process for liquefying coal WO1981000720A1 (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
GB8111221A GB2075046B (en) 1979-09-11 1979-09-11 Process for liquefying coal
PCT/JP1979/000242 WO1981000720A1 (en) 1979-09-11 1979-09-11 Process for liquefying coal
DE792953810A DE2953810C1 (en) 1979-09-11 1979-09-11 PROCESS FOR LIQUEFYING COAL
DK106081A DK161600B (en) 1979-09-11 1981-03-09 PROCEDURE FOR FLUATING COAL

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
PCT/JP1979/000242 WO1981000720A1 (en) 1979-09-11 1979-09-11 Process for liquefying coal
WOJP79/00242 1979-09-11

Publications (1)

Publication Number Publication Date
WO1981000720A1 true WO1981000720A1 (en) 1981-03-19

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DE (1) DE2953810C1 (en)
DK (1) DK161600B (en)
GB (1) GB2075046B (en)
WO (1) WO1981000720A1 (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2464985A1 (en) * 1979-09-12 1981-03-20 Kunitoshi Shimizu Oil prodn. by liquefaction of coal - by agitation with aq. alkali
AU573573B2 (en) * 1983-03-03 1988-06-16 Pentanyl Technologies Inc. Ionic liquefaction
SG11201804901WA (en) 2015-12-22 2018-07-30 SHY Therapeutics LLC Compounds for the treatment of cancer and inflammatory disease

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JPS53108106A (en) * 1977-03-04 1978-09-20 Kunitoshi Shimizu Liquefaction of coal

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GB2075046B (en) 1983-08-24
GB2075046A (en) 1981-11-11
DK161600B (en) 1991-07-22
DK106081A (en) 1981-03-19
DE2953810C1 (en) 1982-02-04

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