JP2017095619A - Method for producing ashless coals - Google Patents

Method for producing ashless coals Download PDF

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JP2017095619A
JP2017095619A JP2015230140A JP2015230140A JP2017095619A JP 2017095619 A JP2017095619 A JP 2017095619A JP 2015230140 A JP2015230140 A JP 2015230140A JP 2015230140 A JP2015230140 A JP 2015230140A JP 2017095619 A JP2017095619 A JP 2017095619A
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coal
solvent
extraction
extraction solvent
pulverized product
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JP6454260B2 (en
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康爾 堺
Koji Sakai
康爾 堺
憲幸 奥山
Noriyuki Okuyama
憲幸 奥山
吉田　拓也
Takuya Yoshida
拓也 吉田
繁 木下
Shigeru Kinoshita
繁 木下
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Kobe Steel Ltd
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Priority to KR1020187017518A priority patent/KR102177978B1/en
Priority to PCT/JP2016/083189 priority patent/WO2017090429A1/en
Priority to CA3002511A priority patent/CA3002511A1/en
Priority to AU2016360026A priority patent/AU2016360026B2/en
Priority to US15/772,265 priority patent/US20180320097A1/en
Priority to CN201680067329.7A priority patent/CN108291164B/en
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    • C10L9/00—Treating solid fuels to improve their combustion
    • C10L9/10—Treating solid fuels to improve their combustion by using additives
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    • C10L2250/00—Structural features of fuel components or fuel compositions, either in solid, liquid or gaseous state
    • C10L2250/06—Particle, bubble or droplet size
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/12—Regeneration of a solvent, catalyst, adsorbent or any other component used to treat or prepare a fuel
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/24—Mixing, stirring of fuel components
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10L2290/28—Cutting, disintegrating, shredding or grinding
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    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/54—Specific separation steps for separating fractions, components or impurities during preparation or upgrading of a fuel
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Abstract

PROBLEM TO BE SOLVED: To provide a method for producing ashless coals, which can make extractability from coal relatively larger.SOLUTION: A method for producing ashless coal comprises: a step S1 for pulverizing coal in the presence of a protective solvent; a step S2 for heating an extraction solvent; a step S3 for mixing a pulverized material obtained at the pulverization step S1 with the extraction solvent obtained at the heating step S2; a step S4 for isolating a solution in which coal components are dissolved, from a slurry obtained at the mixing step S3; and a step S5 for evaporating and separating the protective solvent and the extraction solvent from the solution obtained at the isolation step S4. Preferably in the method for producing the ashless coal, a mean particle diameter of the pulverized material obtained by the pulverizing step S1 is 0.2 mm or lower, and the protective solvent and the extraction solvent are the same solvent. More preferably a content rate of the protective solvent is 20 to 60 mass%.SELECTED DRAWING: Figure 1

Description

本発明は、無灰炭の製造方法に関する。   The present invention relates to a method for producing ashless coal.

火力発電やボイラーの燃料又は化学品の原料として、石炭が幅広く利用されており、環境対策の一つとして石炭中の灰分を効率的に除去する技術の開発が強く望まれている。例えば、ガスタービン燃焼による高効率複合発電システムでは、ＬＮＧ等の液体燃料に代わる燃料として、灰分が除去された無灰炭（ハイパーコール）を使用する試みがなされている。また、高炉用コークス等の製鉄用コークスの原料石炭として無灰炭を使用する試みもなされている。   Coal is widely used as a raw material for thermal power generation and boiler fuel or chemicals, and development of a technology for efficiently removing ash in coal is strongly desired as one of environmental measures. For example, in a high-efficiency combined power generation system using gas turbine combustion, an attempt has been made to use ash-free charcoal (hyper coal) from which ash has been removed as a fuel to replace liquid fuel such as LNG. Attempts have also been made to use ashless coal as the raw coal for ironmaking coke such as blast furnace coke.

無灰炭の製造方法としては、石炭と溶剤とを混合したスラリーを加熱することにより石炭中の可溶成分を溶剤中に溶出させ、固液分離により可溶成分が溶け込んだ溶液を取り出して、この溶液から溶剤を蒸発させることで石炭の可溶成分のみを取り出す方法が一般的である。   As a method for producing ashless coal, by heating a slurry in which coal and a solvent are mixed, a soluble component in the coal is eluted in the solvent, and a solution in which the soluble component is dissolved by solid-liquid separation is taken out. A general method is to extract only the soluble components of coal by evaporating the solvent from this solution.

無灰炭の製造に関し、石炭からより多くの成分を溶剤中に溶出させることで、収率を向上し、無灰炭の製造効率を向上することが望まれている。無灰炭の収率を向上する方法としては、予め加熱した溶剤と石炭とを混合し、短時間で石炭の温度を上昇させることによって、石炭中の成分を溶出し易くする技術が提案されている（例えば特開２０１４−２０８７５７号公報参照）。これは、石炭を急速に昇温することで、石炭を構成する分子間の結合を弱めることができ、結果として、通常では溶出するために時間を要する成分を比較的溶出し易くできることによるものと考えられている。   Regarding the production of ashless coal, it is desired to improve the yield and improve the production efficiency of ashless coal by eluting more components from the coal into the solvent. As a method for improving the yield of ashless coal, a technique has been proposed in which a preheated solvent and coal are mixed, and the temperature of the coal is increased in a short time, so that the components in the coal can be easily eluted. (For example, refer to JP2014-208757A). This is due to the fact that by rapidly raising the temperature of coal, the bonds between the molecules constituting the coal can be weakened, and as a result, components that normally require time to elute can be relatively easily eluted. It is considered.

上述のように、高温の溶剤と石炭とを混合する場合であっても、石炭の粒子径が大きいと石炭の中心部まで急速に昇温することができない。このため、上記公報には、粒度が１ｍｍ未満の石炭の重量割合が８０％以上である細かく粉砕された石炭を用いると記載されている。   As described above, even when a high temperature solvent and coal are mixed, if the particle size of the coal is large, the temperature cannot be rapidly increased to the center of the coal. For this reason, the above publication describes that finely pulverized coal in which the weight ratio of coal having a particle size of less than 1 mm is 80% or more is used.

本発明者らは、石炭を平均粒子径０．１ｍｍ程度の粉末状となるまで粉砕することによってより抽出率を向上しようと試みた。しかしながら、石炭を粉末状に粉砕したところ、却って抽出率が低下する現象が確認された。   The inventors of the present invention have tried to improve the extraction rate by pulverizing coal until it becomes a powder having an average particle size of about 0.1 mm. However, when coal was pulverized into powder, a phenomenon was observed in which the extraction rate decreased.

特開２０１４−２０８７５７号公報JP 2014-208757 A

上記事情に鑑みて、本発明は、石炭からの抽出率を比較的大きくできる無灰炭の製造方法を提供することを課題とする。   In view of the above circumstances, an object of the present invention is to provide a method for producing ashless coal that can relatively increase the extraction rate from coal.

本発明者らは、鋭意研究を重ねた結果、石炭を粉末状に粉砕すると、石炭の表面積が増大し、石炭が空気に触れ易くなることによって風化（酸化）が進行し、結果として無灰炭として利用できる成分が減少するために抽出率が低下すると考えるに至った。そこで、石炭を風化させることなく粉砕すれば抽出率を向上して、無灰炭の製造効率を大きくすることができると予想し、本発明を完成させた。   As a result of intensive research, the inventors of the present invention, when coal is pulverized into a powdery state, the surface area of the coal is increased, and weathering (oxidation) proceeds due to the coal being easily exposed to air, resulting in ashless coal. As a result, the extraction rate declined due to a decrease in available components. Therefore, it was predicted that if the coal was pulverized without weathering, the extraction rate could be improved and the production efficiency of ashless coal could be increased, and the present invention was completed.

上記課題を解決するためになされた発明は、石炭を保護溶剤の存在下で粉砕する工程と、抽出溶剤を加熱する工程と、上記粉砕工程で得られる粉砕物及び上記加熱工程で得られる抽出溶剤を混合する工程と、上記混合工程で得られるスラリーから石炭成分が溶解した溶液を分離する工程と、上記分離工程で得られる溶液から上記保護溶剤及び抽出溶剤を蒸発分離する工程とを備える無灰炭の製造方法である。   The invention made to solve the above problems includes a step of pulverizing coal in the presence of a protective solvent, a step of heating the extraction solvent, a pulverized product obtained in the pulverization step, and an extraction solvent obtained in the heating step. An ashless process comprising: a step of separating the solution obtained by dissolving the coal component from the slurry obtained in the mixing step; and a step of evaporating and separating the protective solvent and the extraction solvent from the solution obtained in the separation step. It is a manufacturing method of charcoal.

当該無灰炭の製造方法は、石炭を保護溶剤の存在下で粉砕する工程を備えるので、石炭が空気に触れ難く、風化を抑制しつつ石炭の粒子径を小さくすることができる。このため、無灰炭として有効な成分が損なわれることを抑制し、混合工程で予め加熱した抽出溶剤の熱により石炭の中心部まで急速に昇温することができるので、石炭からの抽出率を比較的大きくすることができる。従って、当該無灰炭の製造方法は、無灰炭を効率よく製造できる。   Since the method for producing ashless coal includes a step of pulverizing coal in the presence of a protective solvent, the coal is difficult to touch the air, and the particle size of the coal can be reduced while suppressing weathering. For this reason, it can suppress that an effective component as ashless coal is impaired, and since it can heat up rapidly to the center of coal with the heat of the extraction solvent heated beforehand at the mixing process, the extraction rate from coal is It can be made relatively large. Therefore, the method for producing ashless coal can produce ashless coal efficiently.

上記粉砕工程で得られる粉砕物の平均粒子径としては、０．２ｍｍ以下が好ましい。このように、上記粉砕工程で得られる粉砕物の平均粒子径を上記上限以下とすることにより、混合工程で石炭粒子の中心部まで急速に昇温することができるので、石炭からの抽出率をより大きくすることができる。なお、「平均粒子径」とは、レーザー回折法により測定される粒度分布において、累積体積が５０％となる粒子径を意味する。   The average particle size of the pulverized product obtained in the pulverization step is preferably 0.2 mm or less. Thus, by setting the average particle diameter of the pulverized product obtained in the pulverization step to the upper limit or less, the temperature can be rapidly raised to the center of the coal particles in the mixing step, so that the extraction rate from coal can be increased. Can be larger. The “average particle size” means a particle size with a cumulative volume of 50% in the particle size distribution measured by the laser diffraction method.

上記混合工程で、粉砕物の昇温速度が６００℃／分以上となるよう上記粉砕物及び抽出溶剤を混合するとよい。このように、上記混合工程で、粉砕物の昇温速度が６００℃／分以上となるよう上記粉砕物及び抽出溶剤を混合することによって、石炭からの抽出率をより確実に大きくすることができる。なお、「粉砕物の昇温速度」とは、混合開始からスラリーの外見温度である抽出溶剤の温度が安定するまで（粉砕物の内部温度と抽出溶剤の温度とが等しくなったと考えられるまで）の時間で、温度が安定した後のスラリーの温度と混合前の粉砕物の温度との差を除した値として算出される。   In the mixing step, the pulverized product and the extraction solvent may be mixed so that the temperature rise rate of the pulverized product is 600 ° C./min or more. Thus, by mixing the pulverized product and the extraction solvent so that the temperature rising rate of the pulverized product is 600 ° C./min or more in the mixing step, the extraction rate from coal can be increased more reliably. . Note that the “temperature rise rate of the pulverized product” means that the temperature of the extraction solvent, which is the apparent temperature of the slurry, is stabilized from the start of mixing (until the internal temperature of the pulverized product and the temperature of the extraction solvent are considered equal). Is calculated as a value obtained by dividing the difference between the temperature of the slurry after the temperature is stabilized and the temperature of the pulverized product before mixing.

上記保護溶剤と抽出溶剤とが同じ溶剤であるとよい。このように、上記保護溶剤と抽出溶剤とが同じ溶剤であることによって、蒸発分離工程で分離回収した溶剤を再度保護溶剤又は抽出溶剤として利用することができる。   The protective solvent and the extraction solvent may be the same solvent. Thus, when the protective solvent and the extraction solvent are the same solvent, the solvent separated and recovered in the evaporative separation step can be used again as the protective solvent or the extraction solvent.

上記粉砕工程における保護溶剤の含有率としては、２０質量％以上６０％質量以下が好ましい。このように、上記粉砕工程における保護溶剤の含有率を上記範囲内とすることによって、粉砕時の風化を確実に防止すると共に、保護溶剤の顕熱の総量を小さくして、混合工程で抽出溶剤に必要とされる熱量を抑制することができる。   The content of the protective solvent in the pulverization step is preferably 20% by mass or more and 60% by mass or less. Thus, by making the content of the protective solvent in the pulverization step within the above range, weathering during pulverization is surely prevented, and the total amount of sensible heat of the protective solvent is reduced, and the extraction solvent is mixed in the mixing step. The amount of heat required for the process can be suppressed.

以上のように、本発明の無灰炭の製造方法は、石炭からの抽出率を比較的大きくすることができる。   As described above, the method for producing ashless coal of the present invention can relatively increase the extraction rate from coal.

本発明の一実施形態の無灰炭の製造方法の手順を示す流れ図である。It is a flowchart which shows the procedure of the manufacturing method of ashless coal of one Embodiment of this invention. 本発明の実施例、対照例及び比較例の抽出率及び石炭粒子径を示すグラフである。It is a graph which shows the extraction rate and coal particle diameter of the Example of this invention, a control example, and a comparative example.

以下、適宜図面を参照しつつ、本発明の実施の形態を詳説する。   Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings as appropriate.

［無灰炭の製造方法］
図１の無灰炭の製造方法は、石炭を保護溶剤の存在下で粉砕する工程＜ステップＳ１：粉砕工程＞と、抽出溶剤を加熱する工程＜ステップＳ２：加熱工程＞と、上記粉砕工程で得られる粉砕物及び上記加熱工程で得られる抽出溶剤を混合する工程＜ステップＳ３：混合工程＞と、上記混合工程で得られるスラリーから石炭成分が溶解した溶液を分離する工程＜ステップＳ４：溶液分離工程＞と、上記分離工程で得られる溶液から上記保護溶剤及び抽出溶剤を蒸発分離する工程＜ステップＳ５：蒸発分離工程＞とを備える。 [Production method of ashless coal]
The ashless coal production method of FIG. 1 includes a step of pulverizing coal in the presence of a protective solvent <step S1: pulverization step>, a step of heating the extraction solvent <step S2: heating step>, and the above pulverization step. The step of mixing the obtained pulverized product and the extraction solvent obtained in the heating step <Step S3: Mixing step> and the step of separating the solution in which the coal component is dissolved from the slurry obtained in the mixing step <Step S4: Solution separation Step> and a step <Step S5: Evaporation Separation Step> of evaporating and separating the protective solvent and the extraction solvent from the solution obtained in the separation step.

＜粉砕工程＞
ステップＳ１の粉砕工程では、石炭を保護溶剤の存在下で粉砕することによって、粉砕した石炭の表面を保護溶剤で覆い、石炭の粉砕により新たに形成される表面（断面）に空気（特に酸素）が接触することを抑制する。 <Crushing process>
In the pulverization step of step S1, the surface of the pulverized coal is covered with the protective solvent by pulverizing the coal in the presence of the protective solvent, and air (particularly oxygen) is formed on the surface (cross section) newly formed by the pulverization of the coal. Suppresses contact.

石炭の粉砕は、例えば遊星ミル、ボールミル、インパクトミル、リングロールミル、ボールレースミル等を用いて行うことができる。   Coal pulverization can be performed using, for example, a planetary mill, a ball mill, an impact mill, a ring roll mill, a ball race mill, or the like.

この粉砕工程では、予め石炭と保護溶剤とを混ぜ合わせたものを粉砕することで石炭の風化をより確実に防止できるが、特にバッチ式のミルを用いる場合には、粉砕の進行と共に石炭と保護溶剤とが混ぜ合わされて、保護溶剤が石炭粒子の表面を覆うようにしてもよい。   In this pulverization process, weathering of coal can be more reliably prevented by pulverizing a mixture of coal and a protective solvent in advance, but when using a batch-type mill, it is possible to protect the coal with the progress of pulverization. A solvent may be mixed so that the protective solvent covers the surface of the coal particles.

また、粉砕工程は、設備コスト及びエネルギーコストの観点から、大気圧下で行うことが好ましい。また、粉砕工程での石炭及び保護溶剤の温度の上限としては、１００℃が好ましく、８０℃がより好ましく、５０℃がさらに好ましい。一方、粉砕工程での石炭及び保護溶剤の温度の下限としては特に限定されないが、不必要に製造コストを押し上げるような冷却はしない方がよい。粉砕工程での石炭及び保護溶剤の温度が上記上限を超える場合、混合工程で石炭を構成する分子間の結合を弱めることができず、抽出率向上効果が不十分となるおそれがある。   Moreover, it is preferable to perform a grinding | pulverization process under atmospheric pressure from a viewpoint of equipment cost and energy cost. Moreover, as an upper limit of the temperature of coal and a protective solvent in a grinding | pulverization process, 100 degreeC is preferable, 80 degreeC is more preferable, and 50 degreeC is further more preferable. On the other hand, although it does not specifically limit as the minimum of the temperature of coal and a protective solvent in a grinding | pulverization process, it is better not to cool so that a manufacturing cost may be unnecessarily pushed up. When the temperature of the coal and the protective solvent in the pulverization process exceeds the above upper limit, the bond between the molecules constituting the coal cannot be weakened in the mixing process, and the extraction rate improving effect may be insufficient.

この粉砕工程で得られる粉砕物の平均粒子径の下限としては、０．０１ｍｍが好ましく、０．０２ｍｍがより好ましい。一方、この粉砕工程で得られる粉砕物の平均粒子径の上限としては、０．２ｍｍが好ましく、０．１ｍｍがより好ましい。粉砕物の平均粒子径が上記下限に満たない場合、石炭の微細化による抽出率向上効果が飽和状態となるので、不必要にコストが増大するおそれがある。逆に、粉砕物の平均粒子径が上記上限を超える場合、抽出率向上効果が不十分となるおそれがあると考えられる。   The lower limit of the average particle size of the pulverized product obtained in this pulverization step is preferably 0.01 mm, and more preferably 0.02 mm. On the other hand, the upper limit of the average particle size of the pulverized product obtained in this pulverization step is preferably 0.2 mm, more preferably 0.1 mm. If the average particle size of the pulverized product is less than the above lower limit, the effect of improving the extraction rate due to the refinement of coal becomes saturated, which may unnecessarily increase the cost. On the contrary, when the average particle diameter of the pulverized product exceeds the above upper limit, the effect of improving the extraction rate may be insufficient.

また、粉砕工程で得られる粉砕物の累積９０体積粒子径の上限としては、０．５ｍｍが好ましく、０．２ｍｍがより好ましい。一方、この粉砕工程で得られる粉砕物の累積９０体積粒子径の下限としては、上記平均粒子径を満たす限り特に限定されない。粉砕物の累積９０体積粒子径が上記上限を超える場合、抽出率向上効果が不十分となるおそれがあると考えられる。   Further, the upper limit of the cumulative 90 volume particle diameter of the pulverized product obtained in the pulverization step is preferably 0.5 mm, and more preferably 0.2 mm. On the other hand, the lower limit of the cumulative 90 volume particle diameter of the pulverized product obtained in this pulverization step is not particularly limited as long as the average particle diameter is satisfied. If the cumulative 90 volume particle diameter of the pulverized product exceeds the above upper limit, the extraction rate improving effect may be insufficient.

（石炭）
当該無灰炭の製造方法において、原料として用いる石炭としては、特に限定されず、様々な品質の石炭を用いることができる。例えば抽出率の高い瀝青炭や、より安価な劣質炭（亜瀝青炭や褐炭）が好適に用いられる。また、複数種類の石炭を混合したものを原料としてもよい。なお、上記石炭は、風乾等により乾燥炭としてもよいが、水分を含んだ状態のものを用いてもよい。 (coal)
In the method for producing ashless coal, the coal used as a raw material is not particularly limited, and various quality coals can be used. For example, bituminous coal with a high extraction rate or cheaper inferior quality coal (subbituminous coal or lignite) is preferably used. Moreover, it is good also considering what mixed multiple types of coal as a raw material. In addition, although the said coal is good also as dry coal by air drying etc., you may use the thing containing a water | moisture content.

（保護溶剤）
粉砕工程において石炭の表面を覆うために用いられる保護溶剤としては、後述する抽出溶剤との相溶性を有し、蒸発分離工程で蒸発分離又は熱分解により除去し得るものであればよく、常温において石炭との親和性が高い（石炭を濡らし易い）ものが好ましい。 (Protective solvent)
The protective solvent used to cover the surface of the coal in the pulverization process may be any solvent that has compatibility with the extraction solvent described later and can be removed by evaporation separation or thermal decomposition in the evaporation separation process. A thing with high affinity with coal (it is easy to wet coal) is preferable.

保護溶剤の２０℃における動粘度の上限としては、１００ｍｍ２／ｓが好ましく、１０ｍｍ２／ｓがより好ましい。一方、保護溶剤の２０℃における動粘度の下限としては、特に限定されない。保護溶剤の２０℃における動粘度が上記上限を超える場合、石炭の表面で膜切れを起こし易くなり、石炭の風化を十分に防止できないおそれがある。なお、「動粘度」とはＪＩＳ−Ｋ２２８３（２０００）に準拠して測定される値である。 The upper limit of the kinematic viscosity at 20 ° C. of protection solvent, preferably 100 mm 2 / s, and more preferably 10 mm 2 / s. On the other hand, the lower limit of the kinematic viscosity at 20 ° C. of the protective solvent is not particularly limited. When the kinematic viscosity at 20 ° C. of the protective solvent exceeds the above upper limit, film breakage tends to occur on the surface of the coal, and coal weathering may not be sufficiently prevented. The “kinematic viscosity” is a value measured according to JIS-K2283 (2000).

このような保護溶剤としては、例えばベンゼン、トルエン、キシレン等の単環芳香族化合物や、ナフタレン、メチルナフタレン、ジメチルナフタレン、トリメチルナフタレン等の２環芳香族化合物などを挙げることができる。   Examples of such a protective solvent include monocyclic aromatic compounds such as benzene, toluene, and xylene, and bicyclic aromatic compounds such as naphthalene, methylnaphthalene, dimethylnaphthalene, and trimethylnaphthalene.

また、保護溶剤には、例えば石炭の濡れ性を向上する界面活性剤等の添加剤が添加されてもよい。これらの添加剤としては、混合工程又は蒸発分離工程で熱分解するものを用いることが、溶剤の再利用を容易にするために好ましい。   In addition, an additive such as a surfactant that improves the wettability of coal may be added to the protective solvent. As these additives, those which are thermally decomposed in the mixing step or the evaporation separation step are preferably used in order to facilitate the reuse of the solvent.

粉砕工程における保護溶剤の無水無灰ベース（ｄａｆ）での含有率（石炭と保護溶剤との合計量に対する保護溶剤の割合）の下限としては、２０質量％が好ましく、３０質量％がより好ましい。一方、粉砕工程における保護溶剤の含有率の上限としては、６０質量％が好ましく、５０質量％がより好ましい。粉砕工程における保護溶剤の含有率が上記下限に満たない場合、石炭の表面を保護溶剤によって覆うことができないことで石炭の風化を十分に防止できないおそれや、粉砕物の流動性が乏しくなることで粉砕物のハンドリングが容易でなくなるおそれがある。逆に、粉砕工程における保護溶剤の含有率が上記上限を超える場合、保護溶剤の顕熱負荷により、後述する混合工程で溶剤に要求される熱量が大きくなることで、無灰炭の生産性が不必要に低下するおそれがある。   The lower limit of the content of the protective solvent in the anhydrous ashless base (daf) in the pulverization step (the ratio of the protective solvent to the total amount of coal and the protective solvent) is preferably 20% by mass, and more preferably 30% by mass. On the other hand, as an upper limit of the content rate of the protective solvent in a grinding | pulverization process, 60 mass% is preferable and 50 mass% is more preferable. If the content of the protective solvent in the pulverization process is less than the above lower limit, the coal surface cannot be covered with the protective solvent, and the weathering of the coal may not be sufficiently prevented, or the fluidity of the pulverized product becomes poor. There is a possibility that handling of the pulverized product may not be easy. On the other hand, when the content of the protective solvent in the pulverization process exceeds the above upper limit, the sensible heat load of the protective solvent increases the amount of heat required for the solvent in the mixing process, which will be described later. May decrease unnecessarily.

この粉砕工程で得られる粉砕物は、後述する混合工程におけるハンドリング性を向上することができるようペースト状であることが好ましい。粉砕物のペーストの３０℃における粘度の下限としては、０．５Ｐａ・ｓが好ましく、１Ｐａ・ｓがより好ましい。一方、粉砕物のペーストの粘度の上限としては、１０００Ｐａ・ｓが好ましく、６００Ｐａ・ｓがより好ましい。粉砕物のペーストの粘度が上記下限に満たない場合と、粉砕物のペーストに含まれる保護溶剤の割合が多過ぎることにより後述する混合工程での昇温速度が不十分となり、抽出率の向上効果が不十分となるおそれがある。逆に、粉砕物のペーストの粘度が上記上限を超える場合、粉砕物のペーストのハンドリングが容易でなくなるおそれがある。   The pulverized product obtained in this pulverization step is preferably in the form of a paste so that the handling properties in the mixing step described later can be improved. The lower limit of the viscosity of the pulverized paste at 30 ° C. is preferably 0.5 Pa · s, more preferably 1 Pa · s. On the other hand, the upper limit of the viscosity of the paste of the pulverized product is preferably 1000 Pa · s, and more preferably 600 Pa · s. When the viscosity of the paste of the pulverized product is less than the above lower limit and the ratio of the protective solvent contained in the paste of the pulverized product is too large, the heating rate in the mixing step described later becomes insufficient, and the effect of improving the extraction rate May become insufficient. Conversely, when the viscosity of the pulverized paste exceeds the upper limit, handling of the pulverized paste may not be easy.

＜加熱工程＞
ステップＳ２の加熱工程では、抽出溶剤を予め加熱する。抽出溶剤の加熱方法としては、特に限定されないが、例えば熱交換器を用いてインラインで加熱する方法を採用することができる。この熱交換器としては、例えば多管式型、プレート型、スパイラル型等の熱交換器が用いられる。 <Heating process>
In the heating step of step S2, the extraction solvent is preheated. A method for heating the extraction solvent is not particularly limited. For example, a method of heating in line using a heat exchanger can be employed. As this heat exchanger, for example, a heat exchanger such as a multi-tube type, a plate type, or a spiral type is used.

（抽出溶剤）
抽出溶剤としては、石炭を溶解するものであれば特に限定されないが、例えばベンゼン、トルエン、キシレン等の単環芳香族化合物や、ナフタレン、メチルナフタレン、ジメチルナフタレン、トリメチルナフタレン等の２環芳香族化合物などを用いることができる。中でも、石炭を乾留してコークスを製造する際の副生油の蒸留油であるメチルナフタレン、ナフタレン等の石炭由来の２環芳香族化合物が好適に用いられる。この２環芳香族化合物は、基本的な構造が石炭の構造分子と類似していることから石炭との親和性が高く、比較的高い抽出率を得ることができる。 (Extraction solvent)
The extraction solvent is not particularly limited as long as it dissolves coal. For example, monocyclic aromatic compounds such as benzene, toluene and xylene, and bicyclic aromatic compounds such as naphthalene, methylnaphthalene, dimethylnaphthalene and trimethylnaphthalene. Etc. can be used. Among them, bicyclic aromatic compounds derived from coal such as methylnaphthalene and naphthalene, which are distilled oils of by-products when carbonizing carbon to produce coke, are preferably used. Since this bicyclic aromatic compound has a basic structure similar to the structural molecule of coal, it has a high affinity with coal and can obtain a relatively high extraction rate.

また、抽出溶剤は、上記保護溶剤と同じ溶剤であることが好ましい。保護溶剤と抽出溶剤とが同じ溶剤であれば、後述する蒸発分離工程で分離回収した溶剤を、保護溶剤及び抽出溶剤としてそのまま再利用できるので、無灰炭の製造コストを低減することができる。   The extraction solvent is preferably the same solvent as the protective solvent. If the protective solvent and the extraction solvent are the same solvent, the solvent separated and recovered in the evaporative separation step described later can be reused as it is as the protective solvent and the extraction solvent, so that the production cost of ashless coal can be reduced.

抽出溶剤の沸点は、特に限定されないが、例えば抽出溶剤の沸点の下限としては、１８０℃が好ましく、２３０℃がより好ましい。一方、抽出溶剤の沸点の上限としては、３００℃が好ましく、２８０℃がより好ましい。抽出溶剤の沸点が上記下限に満たない場合、後述する蒸発分離工程で抽出溶剤を回収する際の損失が大きくなり、抽出溶剤の回収率が低下するおそれがある。逆に、抽出溶剤の沸点が上記上限を超える場合、溶剤可溶成分と抽出溶剤との分離が困難となり、やはり抽出溶剤の回収率が低下するおそれがある。   The boiling point of the extraction solvent is not particularly limited, but for example, the lower limit of the boiling point of the extraction solvent is preferably 180 ° C and more preferably 230 ° C. On the other hand, the upper limit of the boiling point of the extraction solvent is preferably 300 ° C and more preferably 280 ° C. When the boiling point of the extraction solvent is less than the above lower limit, the loss in recovering the extraction solvent in the evaporation separation step described later increases, and the recovery rate of the extraction solvent may be reduced. Conversely, when the boiling point of the extraction solvent exceeds the above upper limit, it becomes difficult to separate the solvent-soluble component and the extraction solvent, and the recovery rate of the extraction solvent may also decrease.

抽出溶剤の加熱後の温度の下限としては、３３０℃が好ましく、３８０℃がより好ましい。一方、抽出溶剤の加熱後の温度の上限としては、４５０℃が好ましく、４３０℃がより好ましい。抽出溶剤の加熱後の温度が上記下限に満たない場合、後述する混合工程で石炭の粉砕物を十分に昇温することができないことにより、抽出率が不十分となるおそれがある。逆に、抽出溶剤の加熱後の温度が上記上限を超える場合、混合工程で石炭の熱分解反応により生成した熱分解ラジカルの再結合が起こることにより、やはり抽出率が低下するおそれがある。   As a minimum of the temperature after heating of an extraction solvent, 330 ° C is preferred and 380 ° C is more preferred. On the other hand, the upper limit of the temperature after heating the extraction solvent is preferably 450 ° C. and more preferably 430 ° C. When the temperature of the extraction solvent after heating is less than the lower limit, the extraction rate may be insufficient because the coal pulverized product cannot be sufficiently heated in the mixing step described later. On the other hand, when the temperature after heating the extraction solvent exceeds the above upper limit, recombination of pyrolysis radicals generated by the pyrolysis reaction of coal in the mixing step may occur, which may also reduce the extraction rate.

＜混合工程＞
ステップＳ３の混合工程では、上記粉砕工程で得られる保護溶剤を含む粉砕物と、上記加熱工程で加熱した高温の抽出溶剤とを混合することにより、粉砕物中の各石炭粒子の温度を急速に上昇させる。これにより、抽出溶剤中に石炭粒子が分散されたスラリーが得られる。 <Mixing process>
In the mixing step of Step S3, the temperature of each coal particle in the pulverized product is rapidly increased by mixing the pulverized product containing the protective solvent obtained in the pulverizing step and the high temperature extraction solvent heated in the heating step. Raise. Thereby, the slurry by which the coal particle was disperse | distributed in the extraction solvent is obtained.

混合工程における粉砕物の昇温速度の下限としては、６００℃／分が好ましく、１，０００℃／分がより好ましい。一方、混合工程における粉砕物の昇温速度の上限としては、特に限定されないが、２００，０００℃／分が好ましく、１００，００００℃／分がより好ましい。混合工程における粉砕物の昇温速度が上記下限に満たない場合、急速昇温による抽出率の向上効果が不十分となるおそれがある。逆に、混合工程における粉砕物の昇温速度が上記上限を超える場合、処理量が過度に制限されるおそれや、設備コストが不必要に増大するおそれがある。   The lower limit of the temperature rising rate of the pulverized product in the mixing step is preferably 600 ° C./min, and more preferably 1,000 ° C./min. On the other hand, the upper limit of the temperature rising rate of the pulverized product in the mixing step is not particularly limited, but is preferably 200,000 ° C./min, and more preferably 100,000 0000 ° C./min. When the temperature increase rate of the pulverized product in the mixing step is less than the lower limit, the effect of improving the extraction rate due to rapid temperature increase may be insufficient. On the other hand, when the rate of temperature rise of the pulverized product in the mixing step exceeds the above upper limit, the processing amount may be excessively limited or the equipment cost may increase unnecessarily.

粉砕物と抽出溶剤とを混合する方法としては、例えば特開２０１４−２０８７５７号公報に開示されるように、抽出溶剤が流れる配管にロックホッパーで加圧した粉砕物を導入する方法が挙げられる。配管に粉砕物を導入する方法としては、上記ロックホッパーを用いる方法の他にも、例えばポンプを用いる方法等を適用することもできる。   As a method of mixing the pulverized product and the extraction solvent, for example, as disclosed in Japanese Patent Application Laid-Open No. 2014-208757, there is a method of introducing the pulverized product pressurized by a lock hopper into a pipe through which the extraction solvent flows. As a method for introducing the pulverized material into the pipe, in addition to the method using the lock hopper, for example, a method using a pump can be applied.

上記ロックホッパーを用いる方法とは、ガスを供給して内部を加圧できるホッパーにペースト状の粉砕物を収容し、密閉されるホッパーにガスを供給して内部を加圧して、ガスの圧力によりペースト状の粉砕物を押し込む方法である。このロックホッパーは、２つのバルブで区画される配管の一部であってもよい。   The above-mentioned method using a lock hopper is that a paste-like pulverized material is accommodated in a hopper capable of supplying gas and pressurizing the inside, supplying gas to a sealed hopper, pressurizing the inside, and This is a method of pushing a paste-like pulverized product. This lock hopper may be a part of piping divided by two valves.

また、上記ポンプを用いる方法において使用できるポンプとしては、例えばモーノポンプ、サインポンプ、ダイヤフラムポンプ、ベローズポンプ、ロータリーポンプ等が挙げられる。   Examples of the pump that can be used in the method using the pump include a MONO pump, a sine pump, a diaphragm pump, a bellows pump, and a rotary pump.

また粉砕物と抽出溶剤とを混合する方法としては、十分な撹拌能力を有する攪拌機を備え、抽出溶剤を貯留するタンクに粉砕物を一度に投入する方法を採用してもよい。また、粉砕物を入れたタンクに抽出溶剤を一度に投入して撹拌してもよい。   Further, as a method of mixing the pulverized product and the extraction solvent, a method may be adopted in which an agitator having sufficient stirring ability is provided and the pulverized product is put into a tank storing the extraction solvent at a time. Alternatively, the extraction solvent may be charged at once into a tank containing the pulverized product and stirred.

粉砕物と混合される抽出溶剤量の下限としては、粉砕物中の石炭の質量の２倍が好ましく、３倍がより好ましい。一方、粉砕物と混合される抽出溶剤量の上限としては、粉砕物中の石炭の質量の１０倍が好ましく、８倍がより好ましい。粉砕物と混合される抽出溶剤量が上記下限に満たない場合、石炭の成分を十分に抽出することができないおそれがある。逆に、粉砕物と混合される抽出溶剤量が上記上限を超える場合、溶液中の無灰炭成分濃度が低下することにより製造効率が不必要に低下するおそれがある。   The lower limit of the amount of extraction solvent mixed with the pulverized product is preferably 2 times the mass of coal in the pulverized product, and more preferably 3 times. On the other hand, the upper limit of the amount of the extraction solvent mixed with the pulverized product is preferably 10 times the mass of coal in the pulverized product, and more preferably 8 times. When the amount of the extraction solvent mixed with the pulverized product is less than the above lower limit, the coal components may not be sufficiently extracted. On the other hand, when the amount of the extraction solvent mixed with the pulverized product exceeds the above upper limit, the production efficiency may be unnecessarily lowered due to the decrease in the ashless coal component concentration in the solution.

また、粉砕物と混合される抽出溶剤量の粉砕物中の保護溶剤の質量に対する比の下限としては、３倍が好ましく、４倍がより好ましい。一方、粉砕物と混合される抽出溶剤量の粉砕物中の保護溶剤の質量に対する比の上限としては、１５倍が好ましく、１２倍がより好ましい。上記抽出溶剤量と保護溶剤量との比が上記下限に満たない場合、保護溶剤を加熱するための顕熱負荷により石炭粉砕物の昇温速度が不十分となるおそれがある。逆に、上記抽出溶剤量と保護溶剤量との比が上記上限を超える場合、溶液中の無灰炭成分濃度が低下することにより製造効率が不必要に低下するおそれがある。   Further, the lower limit of the ratio of the amount of the extraction solvent mixed with the pulverized product to the mass of the protective solvent in the pulverized product is preferably 3 times, more preferably 4 times. On the other hand, the upper limit of the ratio of the amount of the extraction solvent mixed with the pulverized product to the mass of the protective solvent in the pulverized product is preferably 15 times, and more preferably 12 times. When the ratio of the amount of the extraction solvent and the amount of the protective solvent is less than the lower limit, there is a possibility that the temperature rising rate of the pulverized coal becomes insufficient due to the sensible heat load for heating the protective solvent. On the contrary, when the ratio of the amount of the extraction solvent and the amount of the protective solvent exceeds the above upper limit, the production efficiency may be unnecessarily lowered due to a decrease in the ashless coal component concentration in the solution.

この混合工程で得られるスラリーの温度（石炭粉砕物の温度と同義）の下限としては、３００℃が好ましく、３５０℃がより好ましい。一方、上記スラリーの温度の上限としては、４５０℃が好ましく、４００℃がより好ましい。上記スラリーの温度が上記下限に満たない場合、石炭を構成する分子間の結合を十分に弱めることができないため、抽出率が低下するおそれがある。逆に、上記スラリーの温度が上記上限を超える場合、石炭の熱分解反応が非常に活発になり生成した熱分解ラジカルの再結合が起こるため、抽出率が低下するおそれがある。   As a minimum of the temperature (synonymous with the temperature of coal pulverized material) of the slurry obtained by this mixing process, 300 ° C is preferred and 350 ° C is more preferred. On the other hand, the upper limit of the temperature of the slurry is preferably 450 ° C, more preferably 400 ° C. When the temperature of the slurry is less than the lower limit, the extraction between the molecules constituting the coal cannot be sufficiently weakened, and the extraction rate may be reduced. On the other hand, when the temperature of the slurry exceeds the upper limit, coal pyrolysis reaction becomes very active and recombination of generated pyrolysis radicals occurs, which may reduce the extraction rate.

混合工程で得られたスラリーは、一定時間その温度（抽出温度）を保持して石炭の成分が溶出するのを待つことが好ましい。抽出溶剤が流れる配管に加圧した粉砕物を導入することで粉砕物と抽出溶剤とを混合場合、スラリーを撹拌機を備える抽出槽（タンク）に導入し、この抽出槽で一定時間スラリーを貯留することで、石炭の可溶成分を溶出させるとよい。また、上記抽出温度は、上記混合工程で得られるスラリーの温度であることが好ましいが、制御の容易化やエネルギーコストの低減のために、上記混合工程で得られるスラリーの温度と僅かに異なる温度としてもよい。   The slurry obtained in the mixing step is preferably kept at that temperature (extraction temperature) for a certain time to wait for the coal components to elute. When the pulverized material and the extraction solvent are mixed by introducing pressurized pulverized material into the piping through which the extraction solvent flows, the slurry is introduced into an extraction tank (tank) equipped with a stirrer, and the slurry is stored in this extraction tank for a certain period of time. By doing so, it is good to elute the soluble component of coal. The extraction temperature is preferably the temperature of the slurry obtained in the mixing step. However, in order to facilitate control and reduce energy costs, the extraction temperature is slightly different from the temperature of the slurry obtained in the mixing step. It is good.

この温度保持時間（抽出時間）の下限としては、５分が好ましく、２０分がより好ましい。一方、上記温度保持時間の上限としては、３時間が好ましく、２時間がより好ましい。温度保持時間が上記下限に満たない場合、抽出率が不十分となるおそれがある。逆に、温度保持時間が上記上限を超える場合、サイクルタイムが長くなることで製造効率が不必要に低下するおそれがある。   As a minimum of this temperature holding time (extraction time), 5 minutes are preferable and 20 minutes are more preferable. On the other hand, the upper limit of the temperature holding time is preferably 3 hours, and more preferably 2 hours. If the temperature holding time is less than the lower limit, the extraction rate may be insufficient. On the other hand, when the temperature holding time exceeds the above upper limit, the cycle time becomes long and the production efficiency may be unnecessarily lowered.

粉砕物と抽出溶剤との混合及び得られるスラリーの温度保持は、非酸化性雰囲気で行うことが好ましい。具体的には、スラリーの混合及び温度保持を窒素等の不活性ガスの存在下で行うことが好ましい。窒素等の不活性ガスを用いることで、混合及び温度保持の際にスラリーが酸素に接触して発火することを防止できる。   The mixing of the pulverized product and the extraction solvent and maintaining the temperature of the resulting slurry are preferably performed in a non-oxidizing atmosphere. Specifically, it is preferable to mix the slurry and maintain the temperature in the presence of an inert gas such as nitrogen. By using an inert gas such as nitrogen, the slurry can be prevented from igniting in contact with oxygen during mixing and temperature holding.

粉砕物と抽出溶剤との混合及び得られるスラリーの温度保持の際の圧力は、温度や用いる抽出溶剤の蒸気圧にもよるが、例えば１ＭＰａ以上３ＭＰａ以下とすることができる。混合工程での圧力が抽出溶剤の蒸気圧より低い場合には、抽出溶剤が揮発して石炭中の可溶成分を十分に抽出することができないおそれがある。一方、加熱抽出時の圧力が高すぎると、製造装置の設備コスト及び運転コストが上昇する。   The pressure at the time of mixing the pulverized product and the extraction solvent and maintaining the temperature of the resulting slurry depends on the temperature and the vapor pressure of the extraction solvent used, but can be, for example, 1 MPa or more and 3 MPa or less. If the pressure in the mixing step is lower than the vapor pressure of the extraction solvent, the extraction solvent may volatilize and the soluble components in the coal may not be sufficiently extracted. On the other hand, when the pressure at the time of heating extraction is too high, the equipment cost and the operating cost of the manufacturing apparatus increase.

＜溶液分離工程＞
ステップＳ４の溶液分離工程では、上記混合工程で得られるスラリーを石炭の可溶成分が溶解した溶液を、石炭の不溶成分からなる固形分から分離する。この溶液分離工程では、完全な固液分離は要求されないが、固形分を実質的に含まない溶液をできるだけ多く分離することが望ましい。この溶液を分離する方法としては、例えば重力沈降法、濾過法、遠心分離法等が挙げられ、中でも連続処理に適した重力沈降法が好適に用いられる。重力沈降法では、スラリー中の固形分を重力によって沈降させ、固形分を実質的に含まない上澄液と、固形分が沈殿して形成される固形分濃縮液とに分離する。 <Solution separation process>
In the solution separation step of Step S4, the solution obtained by dissolving the soluble component of coal in the slurry obtained in the mixing step is separated from the solid content of the insoluble component of coal. In this solution separation step, complete solid-liquid separation is not required, but it is desirable to separate as much as possible a solution substantially free of solids. Examples of the method for separating the solution include a gravity sedimentation method, a filtration method, a centrifugal separation method, and the like. Among them, a gravity sedimentation method suitable for continuous treatment is preferably used. In the gravity sedimentation method, solid content in a slurry is settled by gravity, and separated into a supernatant liquid substantially free of solid content and a solid content concentrate formed by precipitation of the solid content.

＜蒸発分離工程＞
ステップＳ５の蒸発分離工程では、溶液分離工程で分離された溶液から保護溶剤及び抽出溶剤を蒸発分離して無灰炭（ハイパーコール）を得る。 <Evaporation separation process>
In the evaporative separation process of step S5, the protective solvent and the extraction solvent are evaporated and separated from the solution separated in the solution separation process to obtain ashless coal (hypercoal).

石炭の可溶成分が溶解した溶液から抽出溶剤及び保護溶剤を蒸発分離する方法としては、例えば蒸留法、蒸発法（スプレードライ法等）等の公知の分離方法を用いることができる。この蒸発分離工程において、溶液から分離された抽出溶剤及び保護溶剤を回収することで、抽出溶剤及び保護溶剤の少なくとも一部として繰り返し使用することができる。   As a method for evaporating and separating the extraction solvent and the protective solvent from the solution in which the soluble component of coal is dissolved, for example, a known separation method such as a distillation method or an evaporation method (spray drying method or the like) can be used. In this evaporative separation step, the extraction solvent and the protective solvent separated from the solution are recovered, so that they can be repeatedly used as at least a part of the extraction solvent and the protective solvent.

このように得られる無灰炭は、灰分が５質量％以下又は３質量％以下であり、灰分を殆ど含まず、水分は皆無であり、また例えば原料石炭よりも高い発熱量を示す。さらに無灰炭は、製鉄用コークスの原料として特に重要な品質である軟化溶融性が大幅に改善され、例えば原料石炭よりも遥かに優れた流動性を示す。従って、当該無灰炭の製造方法によって得られる無灰炭は、コークス原料の配合炭として好適に使用することができる。   The ashless coal thus obtained has an ash content of 5% by mass or less or 3% by mass or less, contains almost no ash, has no moisture, and exhibits a higher calorific value than, for example, raw coal. Furthermore, ashless coal has a significantly improved softening and melting property, which is a particularly important quality as a raw material for iron-making coke, and exhibits fluidity far superior to, for example, raw material coal. Therefore, the ashless coal obtained by the method for producing ashless coal can be suitably used as a blended coal for coke raw materials.

＜利点＞
当該無灰炭の製造方法は、粉砕工程において、石炭を保護溶剤の存在下で粉砕するので、石炭が空気に触れ難く、風化を抑制しつつ石炭の粒子径を小さくすることができる。このため、無灰炭として有効な成分を損なうことなく、混合工程で予め加熱した抽出溶剤の熱により石炭の中心部まで急速に昇温できるので、石炭からの抽出率を比較的大きくすることができる。従って、当該無灰炭の製造方法は、無灰炭を効率よく製造することができる。 <Advantages>
In the ashless coal production method, the coal is pulverized in the presence of a protective solvent in the pulverization step, so the coal is difficult to touch the air, and the particle size of the coal can be reduced while suppressing weathering. For this reason, since the temperature of the coal can be rapidly raised by the heat of the extraction solvent preheated in the mixing step without impairing the components effective as ashless coal, the extraction rate from coal can be made relatively large. it can. Therefore, the manufacturing method of the ashless coal can manufacture ashless coal efficiently.

［その他の実施形態］
上記実施形態は、本発明の構成を限定するものではない。従って、上記実施形態は、本明細書の記載及び技術常識に基づいて上記実施形態各部の構成要素の省略、置換又は追加が可能であり、それらは全て本発明の範囲に属するものと解釈されるべきである。 [Other Embodiments]
The said embodiment does not limit the structure of this invention. Therefore, in the above-described embodiment, the components of each part of the above-described embodiment can be omitted, replaced, or added based on the description and common general knowledge of the present specification, and they are all interpreted as belonging to the scope of the present invention. Should.

以下、実施例に基づき本発明を詳述するが、この実施例の記載に基づいて本発明が限定的に解釈されるものではない。   EXAMPLES Hereinafter, although this invention is explained in full detail based on an Example, this invention is not interpreted limitedly based on description of this Example.

（実施例）
原料となる石炭として平均粒子径０．３ｍｍに予備粉砕した瀝青炭を用い、保護溶剤及び抽出溶剤として１−メチルナフタレンを用いて、本発明の無灰炭の製造方法により無灰炭を試作した。 (Example)
Ashless coal was produced by trial using the method for producing ashless coal of the present invention, using bituminous coal pre-ground to an average particle size of 0.3 mm as the raw material coal and 1-methylnaphthalene as the protective solvent and extraction solvent.

先ず、石炭３０ｇと、保護溶剤２０ｇとを混合してペースト状の混合物を調整した。この混合物を遊星ミルに投入し、混合物中の石炭を平均粒子径０．０４ｍｍになるよう二次粉砕してペースト状の粉砕物を得た。   First, 30 g of coal and 20 g of protective solvent were mixed to prepare a paste-like mixture. This mixture was put into a planetary mill, and the coal in the mixture was secondarily pulverized so as to have an average particle size of 0.04 mm to obtain a paste-like pulverized product.

抽出溶剤１６０ｇを、ステンレスフィルターを有する容量５００ｃｃの加熱圧力装置に投入し、２．０ＭＰａの圧力条件下で４００℃に加熱した。   160 g of the extraction solvent was put into a 500 cc heating pressure device having a stainless steel filter and heated to 400 ° C. under a pressure condition of 2.0 MPa.

この加熱した抽出溶剤に、上記粉砕物を投入し、瞬間的に混合して３８０℃のスラリーを得た。この時の粉砕物の昇温速度は、約１５００℃／分であった。   The pulverized material was charged into the heated extraction solvent and mixed instantaneously to obtain a slurry at 380 ° C. The temperature rising rate of the pulverized product at this time was about 1500 ° C./min.

このスラリーを３８０℃で１時間保持してから、上記加熱圧力装置のステンレスフィルターで濾過して、石炭の可溶成分が溶解した溶液と、石炭の未溶解成分の濾残（固形分）とに分離した。   After holding this slurry at 380 ° C. for 1 hour, the slurry is filtered through a stainless steel filter of the heating pressure device to obtain a solution in which soluble components of coal are dissolved and a filter residue (solid content) of undissolved components of coal. separated.

上記溶液を乾燥して、本発明の実施例による無灰炭を得た。また、上記濾残を乾燥して重量を測定することにより、本発明の実施例における石炭からの可溶成分の抽出率を無水無灰ベース（ｄａｆ）の質量％で算出した。   The above solution was dried to obtain ashless coal according to an example of the present invention. Moreover, the extraction rate of the soluble component from coal in the Example of this invention was computed by the mass% of anhydrous ashless base (daf) by drying the said filter residue and measuring a weight.

（対照例）
比較例として、従来の石炭を急速昇温させる製造方法により無灰炭を試作した。この比較例は、石炭及び保護溶剤の混合物を二次粉砕せずに使用したこと以外は、上記実施例と同じ条件で無灰炭を試作し、石炭からの可溶成分の抽出率を算出した。 (Control example)
As a comparative example, ashless coal was prototyped by a conventional method for rapidly raising the temperature of coal. In this comparative example, an ashless coal was prototyped under the same conditions as in the above example except that a mixture of coal and a protective solvent was used without secondary pulverization, and the extraction rate of soluble components from the coal was calculated. .

（比較例１）
比較例１として、保護溶剤を加えずに石炭をすり鉢を用いて平均粒子径０．０６ｍｍに粉砕し、この粉砕物に保護溶剤を混合してペースト状の粉砕物を得た以外は、上記実施例と同じ条件で無灰炭を試作し、石炭からの可溶成分の抽出率を算出した。 (Comparative Example 1)
As Comparative Example 1, the coal was crushed to an average particle size of 0.06 mm using a mortar without adding a protective solvent, and the protective solvent was mixed with this pulverized product to obtain a paste-like pulverized product. An ashless coal was made under the same conditions as in the example, and the extraction rate of soluble components from the coal was calculated.

（比較例２）
比較例２として、石炭を二次粉砕することなく、常温の抽出溶剤１８０ｇと混合してスラリーを得、このスラリーを加熱圧力装置を用いて昇温速度５．５℃／分で３８０℃まで昇温して１時間保持した以外は、上記実施例と同じ条件で無灰炭を試作し、石炭からの可溶成分の抽出率を算出した。この比較例は、石炭を急速昇温させる製造方法が確立される以前から行われていた一般的な無灰炭の製造方法によるものである。 (Comparative Example 2)
As Comparative Example 2, a slurry was obtained by mixing with 180 g of a normal temperature extraction solvent without secondary pulverization of coal, and this slurry was increased to 380 ° C. at a heating rate of 5.5 ° C./min using a heating pressure device. Except for heating and holding for 1 hour, ashless coal was prototyped under the same conditions as in the above examples, and the extraction rate of soluble components from the coal was calculated. This comparative example is based on a general method for producing ashless coal, which has been performed before the production method for rapidly heating coal is established.

（比較例３）
比較例３として、石炭と保護溶剤との混合物を遊星ミルで粉砕して得たペーストを常温の抽出溶剤１６０ｇと混合してスラリーを得、このスラリーを加熱圧力装置を用いて昇温速度５．５℃／分で３８０℃まで昇温して１時間保持した以外は、上記実施例と同じ条件で無灰炭を試作し、石炭からの可溶成分の抽出率を算出した。 (Comparative Example 3)
As Comparative Example 3, a paste obtained by pulverizing a mixture of coal and a protective solvent with a planetary mill was mixed with 160 g of a normal temperature extraction solvent to obtain a slurry, and this slurry was heated at a rate of temperature increase of 5. Except that the temperature was raised to 380 ° C. at 5 ° C./min and held for 1 hour, ashless coal was prototyped under the same conditions as in the above examples, and the extraction rate of soluble components from the coal was calculated.

（比較例４）
比較例４として、保護溶剤を加えずに石炭をすり鉢を用いて平均粒子径０．０６ｍｍに粉砕したものと常温の抽出溶剤１８０ｇとを混合してスラリーを得、このスラリーを加熱圧力装置を用いて昇温速度５．５℃／分で３８０℃まで昇温して１時間保持した以外は、上記実施例と同じ条件で無灰炭を試作し、石炭からの可溶成分の抽出率を算出した。 (Comparative Example 4)
As Comparative Example 4, coal was pulverized to an average particle size of 0.06 mm using a mortar without adding a protective solvent and 180 g of a normal temperature extraction solvent was mixed to obtain a slurry, and this slurry was heated using a heating pressure device. The ash-free coal was prototyped under the same conditions as in the above example except that the temperature was raised to 380 ° C. at a heating rate of 5.5 ° C./min and held for 1 hour, and the extraction rate of soluble components from the coal was calculated. did.

図２に、上記実施例、対照例及び比較例１〜４の平均粒子径と石炭からの抽出率との関係をまとめて示す。   In FIG. 2, the relationship between the average particle diameter of the said Example, a comparative example, and Comparative Examples 1-4 and the extraction rate from coal is shown collectively.

石炭のペーストを加熱した抽出溶剤と混合して石炭の温度を急速に上昇させた実施例、対照例及び比較例１を比較すると、石炭を二次粉砕しなかった対照例に対して、保護溶剤の存在下で石炭を二次粉砕した実施例は抽出率が向上したが、保護溶剤を加えず空気に触れる状態で石炭を二次粉砕した比較例１は粒子径を小さくしたにも拘わらず抽出率が低下した。   When comparing the example in which the coal paste was mixed with the heated extraction solvent and the temperature of the coal was rapidly increased, the control example and the comparative example 1, the protective solvent was compared with the control example in which the coal was not secondarily pulverized. The extraction rate of the example in which the coal was secondarily pulverized in the presence of NO was improved, but the comparative example 1 in which the coal was secondly pulverized in a state where it was exposed to air without adding a protective solvent was extracted although the particle size was reduced. The rate fell.

また、これら石炭の温度を急速に上昇させた対照例、実施例及び比較例１と、石炭の温度を緩慢に上昇させた比較例２、比較例３及び比較例４とを比較すると、石炭粉砕方法が同じであれば、石炭の温度を急速に上昇させたもの方が石炭の温度を緩慢に上昇させたものよりも高い抽出率が得られた。   Moreover, when the comparative example, Example, and Comparative example 1 which raised the temperature of these coal rapidly, and the comparative example 2, comparative example 3, and comparative example 4 which raised the temperature of coal slowly, coal grinding | pulverization is carried out. If the method was the same, a higher extraction rate was obtained when the coal temperature was increased rapidly than when the coal temperature was increased slowly.

また、石炭の温度を緩慢に上昇させる場合、石炭を粉砕しなかった比較例２と、保護溶剤の存在下で石炭を粉砕した比較例３とでは、抽出率に殆ど差がなく、保護溶剤を加えず石炭を粉砕した比較例４は、比較例２及び比較例３よりも抽出率が低かった。   Moreover, when raising the temperature of coal slowly, there is almost no difference in an extraction rate in the comparative example 2 which did not grind | pulverize coal, and the comparative example 3 which grind | pulverized coal in presence of a protective solvent, and a protective solvent is used. In Comparative Example 4 in which coal was pulverized without addition, the extraction rate was lower than in Comparative Example 2 and Comparative Example 3.

以上の結果から、石炭を保護溶剤の存在下で粉砕することで、石炭中の可溶成分を減少させることなく、加熱した溶剤により石炭を急速に昇温させることで抽出率を向上する効果が大きくできることが確認された。   From the above results, the effect of improving the extraction rate by rapidly heating the coal with the heated solvent without reducing soluble components in the coal by grinding the coal in the presence of a protective solvent. It was confirmed that it could be enlarged.

本発明の無灰炭の製造方法は、例えば燃料、コークス原料等として用いられる無灰炭を製造するために広く利用することができる。   The method for producing ashless coal of the present invention can be widely used for producing ashless coal used as, for example, fuel, coke raw material and the like.

Ｓ１ 粉砕工程
Ｓ２ 加熱工程
Ｓ３ 混合工程
Ｓ４ 溶液分離工程
Ｓ５ 蒸発分離工程 S1 Crushing step S2 Heating step S3 Mixing step S4 Solution separation step S5 Evaporation separation step

Claims (5)

石炭を保護溶剤の存在下で粉砕する工程と、
抽出溶剤を加熱する工程と、
上記粉砕工程で得られる粉砕物及び上記加熱工程で得られる抽出溶剤を混合する工程と、
上記混合工程で得られるスラリーから石炭成分が溶解した溶液を分離する工程と、
上記分離工程で得られる溶液から上記保護溶剤及び抽出溶剤を蒸発分離する工程と
を備える無灰炭の製造方法。 Crushing coal in the presence of a protective solvent;
Heating the extraction solvent;
Mixing the pulverized product obtained in the pulverization step and the extraction solvent obtained in the heating step;
Separating the solution in which the coal component is dissolved from the slurry obtained in the mixing step;
And a step of evaporating and separating the protective solvent and the extraction solvent from the solution obtained in the separation step. 上記粉砕工程で得られる粉砕物の平均粒子径を０．２ｍｍ以下にする請求項１に記載の無灰炭の製造方法。   The method for producing ashless coal according to claim 1, wherein the average particle size of the pulverized product obtained in the pulverization step is 0.2 mm or less. 上記混合工程で、粉砕物の昇温速度が６００℃／分以上となるよう上記粉砕物及び抽出溶剤を混合する請求項１又は請求項２に記載の無灰炭の製造方法。   The method for producing ashless coal according to claim 1 or 2, wherein in the mixing step, the pulverized product and the extraction solvent are mixed so that the temperature rising rate of the pulverized product is 600 ° C / min or more. 上記保護溶剤と抽出溶剤とが同じ溶剤である請求項１、請求項２又は請求項３に記載の無灰炭の製造方法。   The method for producing ashless coal according to claim 1, wherein the protective solvent and the extraction solvent are the same solvent. 上記粉砕工程における保護溶剤の含有率が２０質量％以上６０％質量以下である請求項１から請求項４のいずれか１項に記載の無灰炭の製造方法。   The method for producing ashless coal according to any one of claims 1 to 4, wherein a content of the protective solvent in the pulverization step is 20% by mass or more and 60% by mass or less.
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