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JP6372264B2 - Evaluation method of sinter production process - Google Patents
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JP6372264B2 - Evaluation method of sinter production process - Google Patents

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JP6372264B2
JP6372264B2 JP2014182616A JP2014182616A JP6372264B2 JP 6372264 B2 JP6372264 B2 JP 6372264B2 JP 2014182616 A JP2014182616 A JP 2014182616A JP 2014182616 A JP2014182616 A JP 2014182616A JP 6372264 B2 JP6372264 B2 JP 6372264B2
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康弘 藤部
康弘 藤部
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Nippon Steel Corp
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本発明は、焼結鉱製造工程の評価方法に関し、特に焼結鉱製造工程における焼結鉱強度と焼結鉱生産速度について、大規模実験を用いず、焼結鉱製造工程を模擬した実験によって求められる歩留と燃焼速度から簡便に評価することを可能にする方法に関する。   The present invention relates to a method for evaluating a sinter production process, and in particular, for a sinter strength and a sinter production rate in a sinter production process, by using an experiment simulating the sinter production process without using a large-scale experiment. The present invention relates to a method that enables simple evaluation from required yield and burning rate.

高炉を有する一貫製鉄所では、安価良質の銑鉄を安定的に生産することが最重要項目である。銑鉄を生産する高炉の主原料は鉄鉱石である。鉄鉱石は一般的に粒径により塊鉱(粒径>5mm)と紛鉱(粒径≦5mm)に分類される。通常、紛鉱は塊鉱に比べ、より安価である。しかしながら、粉鉱を高炉に直接投入した場合、炉内を密に充填してしまう。その結果、高炉操業において必須の、下方からの熱風の送風が阻害され、炉内での連続的な還元反応が滞るため、安定した銑鉄の生産を困難にする。   In an integrated steelworks with a blast furnace, the most important item is the stable production of cheap and high-quality pig iron. The main raw material of the blast furnace producing pig iron is iron ore. Iron ore is generally classified into massive ore (particle size> 5 mm) and powder ore (particle size ≦ 5 mm) according to particle size. Usually, ore is cheaper than lump ore. However, when the powder ore is directly charged into the blast furnace, the furnace is densely filled. As a result, the blowing of hot air from below, which is essential in blast furnace operation, is hindered, and the continuous reduction reaction in the furnace is delayed, making stable pig iron production difficult.

そこで、紛鉱を予め一定サイズ以上の粒径を持った焼結鉱として、高温で焼き固める、原料前処理(塊成化)方法が一般的に行われている。上記、焼結鉱に求められる性状としては、前述の塊成化による粒径の向上に加え、ベルトコンベア等での運搬や高炉投入時の衝撃で紛化しない冷間強度が重要な指標となる。   Therefore, a raw material pretreatment (agglomeration) method is generally performed in which powder ore is baked and hardened at a high temperature as a sintered ore having a particle size of a certain size or more in advance. As the properties required for the sintered ore, in addition to the improvement of the particle size due to the agglomeration described above, the cold strength that does not disintegrate due to the impact at the time of transportation on a belt conveyor or the blast furnace is an important index. .

焼結鉱の製造に用いる原料は、主原料の鉄鉱石のほかに、副原料の石灰、珪砂等である。焼結鉱製造工程に投入する際には、あらかじめ、上記の原料と熱源となる固体燃料として粉状のコークス(以下、「粉コークス」と呼ぶ)を、一定の比率で混合し、バインダーとなる水等を加え、回転ドラム等で造粒し焼結疑似粒子を造る。上記、造粒された焼結疑似粒子は、ベルトコンベア状の焼結機パレットに適当な層厚で敷き詰められ連続的に搬送される。搬送の上流部分で、上層にバーナー等を用いて着火、上方の疑似粒子中に内装された固体燃料を燃焼させる。この燃焼熱は焼結機パレットを下方吸引することで伝熱し、順次、疑似粒子層内の固体燃料の着火を起こし、熱伝播が起き、焼結原料全体が焼結される。この際の熱伝播の速度がより早ければ、焼結鉱の生産速度を向上させることができる。   The raw materials used for the production of sintered ore are lime, quartz sand, etc. as auxiliary raw materials in addition to iron ore as the main raw material. When putting into the sinter ore production process, powdery coke (hereinafter referred to as “powder coke”) as a solid fuel that serves as a heat source is mixed with a predetermined ratio in advance to become a binder. Add water, etc., and granulate with a rotating drum etc. to make sintered pseudo particles. The granulated sintered pseudo particles are spread on a belt conveyor-like sintering machine pallet with an appropriate layer thickness and continuously conveyed. In the upstream part of the conveyance, the upper layer is ignited using a burner or the like, and the solid fuel embedded in the upper pseudo particles is burned. This combustion heat is transferred by suctioning the sintering machine pallet downward, and in turn, the solid fuel in the pseudo particle layer is ignited, heat propagation occurs, and the entire sintering raw material is sintered. If the heat propagation speed at this time is faster, the production speed of the sintered ore can be improved.

このような連続搬送と下方吸引を組み合わせた焼結鉱製造工程は安価、簡素なプロセスである。しかし、下方吸引というプロセスの特性上、層内で連続低燃焼が可能な固体燃料を用いる必要がある。従来、この固体燃料としては、製鐵所で製造される高炉用コークスのうち、おおよそ5mm以下の粒径である粉コークスが用いられてきた。しかしながら、近年、石炭チャーやバイオマス等異なる固体燃料が検討されつつある(非特許文献1)。   Such a sinter production process combining continuous conveyance and downward suction is an inexpensive and simple process. However, due to the characteristic of the process of downward suction, it is necessary to use a solid fuel capable of continuous low combustion in the layer. Conventionally, as this solid fuel, among the blast furnace coke produced at the steelworks, powder coke having a particle diameter of approximately 5 mm or less has been used. However, in recent years, different solid fuels such as coal char and biomass are being studied (Non-Patent Document 1).

上記のような異なる熱源の評価を進めるためには、特許文献1や特許文献2に記載されているような鍋試験と呼ばれる大規模実験が行われる。鍋試験では、50kg程度の焼結原料を耐火物を敷き詰めた鍋状炉に投入し、表面部に着火し下方から空気吸引を行う。一般的に各種焼結条件における焼結生産性の評価は、本試験法によって得られた、生産速度、歩留、生産率等から評価される。しかし、このような大規模実験は時間を要し、金銭的に高コストであり、多くの水準で実行する必要がある場合には適していないという課題があった。   In order to proceed with the evaluation of the different heat sources as described above, a large-scale experiment called a pan test as described in Patent Document 1 or Patent Document 2 is performed. In the pot test, about 50 kg of sintered raw material is put into a pot-shaped furnace covered with refractories, ignited on the surface, and air is sucked from below. In general, the evaluation of the sintering productivity under various sintering conditions is evaluated from the production speed, yield, production rate, etc. obtained by this test method. However, such a large-scale experiment has a problem that it takes time, is expensive in money, and is not suitable when it needs to be performed at many levels.

また、特に各種焼結条件のうち、固体燃料に着目すると、固体燃料特有の燃焼性により焼結生産性が変化しうることが知られているが(非特許文献2)、鍋試験では同時に焼結条件である、焼結温度や風量の制御が容易ではないことから、固体燃料の評価のみに焦点を絞って評価することは容易ではなかった。また、鍋試験で得られるのは複雑な焼結反応下の総体としてのマクロ結果であるため、固体燃料の燃焼の特性である燃焼速度や発熱量との相関を明らかにすることができず、焼結工程に適した燃料の解析が容易でないという問題点があった。   In particular, it is known that among various sintering conditions, focusing on solid fuel, it is known that sintering productivity can change due to the combustibility unique to solid fuel (Non-Patent Document 2). Since it is not easy to control the sintering temperature and the air volume, which are the sintering conditions, it was not easy to focus on the evaluation of the solid fuel. In addition, because the pan test results in macro results as a whole under a complex sintering reaction, it is not possible to clarify the correlation with the burning rate and calorific value that are the characteristics of solid fuel combustion, There is a problem that it is not easy to analyze a fuel suitable for the sintering process.

上記の問題点に対し、焼結条件を制御した、低コストの実験室系の焼結実験方法が提案されている(特許文献3)。大型試験に対し、小容量の実験を行うことで、焼結温度や風量が一定下での実験が可能となり、また、試料量を少なくすることで多種の固体燃料の評価が可能となったが、一方で、本装置を用いた場合の焼結鉱製造工程における生産性の評価方法は確立されていなかった。   In order to solve the above problems, a low-cost laboratory-type sintering experiment method in which the sintering conditions are controlled has been proposed (Patent Document 3). By conducting a small-capacity experiment for a large-scale test, it was possible to conduct experiments under a constant sintering temperature and air volume, and it became possible to evaluate various solid fuels by reducing the sample volume. On the other hand, the productivity evaluation method in the sinter manufacturing process when this apparatus is used has not been established.

特開平7−316675号公報JP 7-316675 A 特開2008−19455号公報JP 2008-19455 A 特開2012−255201号公報JP 2012-255201 A

ふぇらむ 鉄鋼協会会誌 Vol.17 No.8 Page.565-572Ferum Steel Association Vol.17 No.8 Page.565-572 鉄鋼協会 高温プロセス部会シンポジウム「低炭素焼結技術原理の創生」研究会 中間報告Interim Report of the High Temperature Process Group Symposium “Creation of Low Carbon Sintering Technology Principle” Study Group

本発明の目的は、従来大型試験を用いてしか行うことができなかった焼結鉱製造工程の評価を、実験室規模の小規模実験に基づいて評価することが可能な手法を提案するとともに、固体燃料の燃焼の特性である燃焼速度や発熱量と焼結生産率や歩留まりとの相関を明らかにして、最適な固体燃料の選択を可能とすることにある。   The purpose of the present invention is to propose a method capable of evaluating the sinter production process, which could only be performed using a large-scale test, based on a small-scale experiment on a laboratory scale, It is intended to make it possible to select an optimal solid fuel by clarifying the correlation between the burning rate and calorific value, which are the characteristics of solid fuel combustion, and the sintering production rate and yield.

本発明者は、大規模実験による焼結鉱製造工程の評価における課題を解決するため、実験室系での小規模な模擬焼結試験に基づいて評価する手法を検討した。その結果、10g以下の焼結試料の焼結歩留、燃焼速度の評価方法を提案するに至った。   The present inventor has studied a method of evaluation based on a small-scale simulated sintering test in a laboratory system in order to solve the problem in the evaluation of the sinter production process by a large-scale experiment. As a result, the inventors have proposed a method for evaluating the sintering yield and burning rate of sintered samples of 10 g or less.

本発明の要旨は以下(1)〜()の通りである。
(1)焼結鉱製造工程の評価方法であって、
〔1〕鉄鉱石原料と固体燃料とを含む0.01g以上10g以下の焼結模擬試料を用いた焼結模擬試験を、前記焼結模擬試料の表面温度をT(K)、焼結に必要な雰囲気ガスの単位時間あたりの送風量をV(m3/s)、前記雰囲気ガスの酸素分圧をPO2(kPa)、として、表面温度T、酸素分圧PO2、送風量Vを予め与えられた値に制御して行う工程と、
〔2〕前記焼結模擬試験時の前記固体燃料の燃焼ガスの測定を行う工程と、
〔3〕前記燃焼ガスの測定結果から燃焼速度を求める工程と、
〔4〕焼結試験後の焼結鉱試料の歩留を求める工程と、
〔5〕前記燃焼速度と前記歩留とから、前記焼結鉱製造工程を評価する工程、
とからなり、
工程〔2〕では、焼結時発生ガス量の時間に対する変化を表すピークの半値幅Δt(s)を求め、
工程〔3〕では、前記燃焼速度として、前記焼結模擬試料の充填高さh(mm)を工程〔2〕で求めた前記ピークの半値幅Δt(s)で除した、下記式(2)の焼結進行速度r(mm/s)を求め、
r=h(mm)/Δt(s) (2)
工程〔4〕では、焼結鉱試料の歩留を、前記焼結模擬試験で得られた全試料のうち、原料粒度より大きくなった試料量S1と原料粒度以下の試料量S2による次の式(1)
P=S1/(S1+S2) (1)
によって求められる塊率Pとして求め、
工程〔5〕では、以下の式(3)
Sv=P×r (3)
により焼結工程の評価値Svを求め、Sv=8を超える評価値を示した固体燃料を、焼結鉱製造工程に好適であると判断する、
ことを特徴とする焼結鉱製造工程の評価方法。
The gist of the present invention is as follows (1) to ( 2 ).
(1) An evaluation method of a sinter production process,
[1] Sintering simulation test using 0.01 g or more and 10 g or less sintering simulated sample containing iron ore raw material and solid fuel, surface temperature of said sintered simulated sample is required for T (K), sintering A surface temperature T, an oxygen partial pressure PO2, and an air flow rate V are given in advance, where V (m 3 / s) is the air flow rate per unit time of the atmospheric gas, and oxygen partial pressure of the atmospheric gas is PO 2 (kPa). A process that is controlled to a specific value,
[2] a step of measuring the combustion gas of the solid fuel during the sintering simulation test;
[3] A step of obtaining a combustion rate from the measurement result of the combustion gas;
[4] A step of obtaining the yield of the sintered ore sample after the sintering test,
[5] A step of evaluating the sinter production process from the burning rate and the yield,
Ri Do not from the,
In the step [2], a half width Δt (s) of a peak representing a change with respect to time of the amount of gas generated during sintering is obtained,
In the step [3], as the burning rate, the filling height h (mm) of the sintered simulation sample is divided by the half-value width Δt (s) of the peak obtained in the step [2]. The sintering progress speed r (mm / s) of
r = h (mm) / Δt (s) (2)
In the step [4], the yield of the sintered ore sample is determined by the following equation based on the sample amount S1 larger than the raw material particle size and the sample amount S2 less than the raw material particle size among all the samples obtained in the sintering simulation test. (1)
P = S1 / (S1 + S2) (1)
Obtained as a mass ratio P obtained by
In step [5], the following formula (3)
Sv = P × r (3)
The evaluation value Sv of the sintering process is obtained by the above, and the solid fuel showing an evaluation value exceeding Sv = 8 is determined to be suitable for the sintered ore production process.
The evaluation method of the sintered ore manufacturing process characterized by the above-mentioned.

)前記焼結模擬試料の量が0.5g以上1g以下であることを特徴とする、(1)に記載の焼結鉱製造工程の評価方法。 ( 2 ) The method for evaluating a sintered ore production process according to (1 ), wherein the amount of the sintered simulation sample is 0.5 g or more and 1 g or less.

焼結鉱製造工程の評価方法として、実験室系での評価を用いることで、従来の大型試験より低コストで実施可能となるので、より多くの実験水準の実施が容易となり、最適な原料、副原料、燃料の選択や、最適な焼結条件の提示が可能となる。また、従来技術による燃焼速度の評価と実機の生産速度や、発熱量の大小と歩留は必ずしも一致しなかったが、本発明は焼結鉱製造工程を模擬した実験を用いることでそれらの評価を可能とする。   As an evaluation method of the sinter production process, it is possible to carry out at a lower cost than conventional large-scale tests by using the evaluation in the laboratory system. It is possible to select auxiliary materials and fuels and to present optimum sintering conditions. In addition, although the evaluation of the burning rate according to the prior art and the production rate of the actual machine, the magnitude of the calorific value, and the yield did not necessarily match, the present invention evaluated them by using an experiment simulating the sinter production process. Is possible.

本発明による焼結模擬試験に用いる装置を模式的に示した図である。It is the figure which showed typically the apparatus used for the sintering simulation test by this invention. 燃焼模擬試験によって得られるガス発生量や温度等の経時変化を示した図である。It is the figure which showed the time-dependent change of the gas generation amount obtained by a combustion simulation test, temperature, etc. 焼結模擬試験によって得られる燃焼速度を求めるための半値幅を示した図である。It is the figure which showed the half value width for calculating | requiring the combustion rate obtained by a sintering simulation test. 本評価法で得られるデータと鍋試験との対応を示した図である。It is the figure which showed the response | compatibility with the data obtained by this evaluation method, and a pan test.

以下に、本発明における焼結鉱製造工程の評価方法の手順を具体的に示す。
本発明における評価手法の手順は概ね次の二つの工程に分けられる。すなわち、第一に、実験室系での焼結鉱製造工程を模擬した試験(以下単に「焼結模擬試験」と呼ぶ)を行い、第二に、試験により得られた結果から焼結鉱製造工程の歩留と燃焼速度を求め、焼結鉱製造工程の生産性の評価を行う。
Below, the procedure of the evaluation method of the sintered ore manufacturing process in this invention is shown concretely.
The procedure of the evaluation method in the present invention is roughly divided into the following two steps. That is, first, a test simulating a sinter production process in a laboratory system (hereinafter simply referred to as “sinter simulation test”) is performed, and second, a sinter production is performed from the results obtained by the test. The process yield and burning rate are obtained, and the productivity of the sinter manufacturing process is evaluated.

まず、第一の焼結模擬試験について、試験に用いる焼結試験装置とその使用方法を具体的に説明する。説明する装置の模式図を図1に示す。本装置の構成は大きく分けて四部分であり、一つ目は実験試料を保持する試料管部分、二つ目は試料管部分と空気吸引するポンプおよびそれらを接続する配管部分、三つ目は試料を加熱、着火する加熱装置部分、四つ目は装置の各所に接続する各種検出器部分である。   First, regarding the first sintering simulation test, a sintering test apparatus used for the test and a method for using the same will be described in detail. A schematic diagram of the apparatus to be described is shown in FIG. The configuration of this equipment is broadly divided into four parts. The first is a sample tube part that holds experimental samples, the second is a sample pipe part and a pump that sucks air and a pipe part that connects them, and the third is The heating device part for heating and igniting the sample, and the fourth part are various detector parts connected to various parts of the apparatus.

本試験では焼結条件を均一に制御することが望ましく、そのため試料量は加熱装置の性能等によって変わりうるが、より少ない方が望ましい。一方で、後段に示す固体試料の評価方法に用いる際の、結果のバラつきを抑制するためには、より多くの試料を用いることが有効である。発明者は、種々検討した結果、燃焼時の条件を制御しつつ、得られる実験結果のバラツキを抑えるためには、試料量(主原料の鉄鉱石および固体燃料と、石灰などのその他の添加物質との合計質量)の上限としては10g以下が妥当であり、より望ましくは1g以下であるとの知見を得た。一方、下限としては、10mg以上が妥当であり、望ましくは500mg以上であるとの知見を得た。   In this test, it is desirable to uniformly control the sintering conditions, and therefore the amount of the sample can vary depending on the performance of the heating device, but it is desirable that the amount is smaller. On the other hand, it is effective to use a larger number of samples in order to suppress variation in results when used in the solid sample evaluation method described later. As a result of various studies, the inventor has controlled the amount of sample (mainly iron ore and solid fuel, and other additive substances such as lime) in order to suppress variations in the experimental results while controlling the combustion conditions. 10 g or less is appropriate as the upper limit of the total mass), and more preferably 1 g or less. On the other hand, as a lower limit, it was found that 10 mg or more is appropriate, and desirably 500 mg or more.

以下、各部分の装置の詳細を示す。
第一に、試料管部分の構成について説明する。まず、試料を保持する部分について、図1の2および3に相当する約1400℃程度の反応温度に耐えることが可能な素材を用い空気吸引可能な中空の試料管を作製する(以下、単に「試料管」と呼ぶ)。材質はSiCや、セラミックス、白金等が使用可能である。また、反応が短時間である場合、安価な石英を用いる事も可能である。この試料保持部の管3の内径は、実験に使用する焼結原料で2mm以上の厚みで、隙間無く充填可能な程度でなければならない。例えば1g以下の焼結原料量にて充填する場合、試料管径は10mm以下が適当である。また、後述するが、燃焼条件となる酸素分圧とガス流速といった、反応雰囲気を制御するため、試料管をさらに大径の容器(図1の4)で内包する。よって必要以上に大径とするのは非効率である。
The details of the apparatus of each part are shown below.
First, the configuration of the sample tube portion will be described. First, a hollow sample tube capable of air suction is prepared using a material that can withstand a reaction temperature of about 1400 ° C. corresponding to 2 and 3 in FIG. Called "sample tube"). As the material, SiC, ceramics, platinum, or the like can be used. In addition, when the reaction is short, inexpensive quartz can be used. The inner diameter of the tube 3 of this sample holding part must be such that the sintered raw material used in the experiment is 2 mm or more thick and can be filled without a gap. For example, when filling with a sintering raw material amount of 1 g or less, the sample tube diameter is suitably 10 mm or less. As will be described later, in order to control the reaction atmosphere, such as oxygen partial pressure and gas flow rate, which are combustion conditions, the sample tube is enclosed in a larger-diameter container (4 in FIG. 1). Therefore, it is inefficient to make the diameter larger than necessary.

試料管の形状は単純な管状構造でも問題ないが、焼結原料を充填する端部2について、ロート状、皿状にすることは試料の適量を安定的に保持可能となり有効である。またそれぞれの形状に加工した場合でも、下方から空気吸引可能とする形状が望ましい。さらに試料管内部をガス吸引によって焼結原料が流れないような形状にすることや、火格子を設置することも有効であるが、市販のグラスウール等によって吸引空気を阻害せず、試料を固定することも可能である。   There is no problem with the shape of the sample tube even if it is a simple tubular structure, but it is effective to make the end portion 2 filled with the sintering raw material into a funnel shape or a dish shape so that an appropriate amount of the sample can be stably held. Further, even when each shape is processed, a shape that allows air suction from below is desirable. It is also effective to make the inside of the sample tube so that the sintering raw material does not flow by gas suction or to install a grate, but the sample is fixed without inhibiting the suction air with commercially available glass wool etc. It is also possible.

第二に、空気吸引を行うポンプおよびそれを前記試料管と接続する配管部分について説明する。装置に用いるポンプは、中空の試料管径に対し、充分な排気量をもっている必要がある。より具体的には、焼結鉱製造過程の一般的な排気速度の0.2〜1.0m/秒と同等とするため、試料管径断面積Sm2に対し下式を満たす排気量Qm3/秒を満たす必要が有る。
0.2(m/秒)<Q(m3/秒)・S(m2
Secondly, a pump that performs air suction and a pipe portion that connects the pump to the sample tube will be described. The pump used in the apparatus needs to have a sufficient displacement with respect to the hollow sample tube diameter. More specifically, in order to make it equal to 0.2 to 1.0 m / sec, which is a general exhaust speed in the sinter production process, the displacement Qm 3 satisfying the following equation with respect to the sample tube diameter cross-sectional area Sm 2 / Sec must be satisfied.
0.2 (m / sec) <Q (m 3 / sec) · S (m 2 )

さらにポンプの排気量についてはコントロールできることが望ましいが、流量を制御できるようなバルブを設置することでも制御対応可能である。   Further, it is desirable that the pump displacement can be controlled, but it is possible to control it by installing a valve capable of controlling the flow rate.

配管部分のうち、試料管とポンプの接続に用いる配管の材質は特に規定されないが、副生ガスに含まれる酸性ガスによる腐食を防ぐ目的で、ステンレス製であることが望ましい。中空試料管と配管の接続方法も特に規定されないが、副生ガスが漏出しないことが必須であり、例えば溶接や、接着剤、熱収縮チューブによる密着などの方法がある。さらに配管同士と各装置の接続もステンレス製の継ぎ手等によって、発生ガスの漏出無きよう接続を行う。   Of the piping parts, the material of the piping used for connecting the sample tube and the pump is not particularly defined, but is preferably made of stainless steel for the purpose of preventing corrosion caused by acid gas contained in the by-product gas. The connection method between the hollow sample tube and the pipe is not particularly specified, but it is essential that the by-product gas does not leak out. For example, there are methods such as welding, adhesion using an adhesive, and a heat shrinkable tube. Further, the pipes and each device are connected by a stainless steel joint so that the generated gas does not leak.

第三に、焼結原料の加熱装置部分について説明する。主たる加熱方法は焼結原料に内装された固体燃料の燃焼熱による内熱方式であり、固体燃料への着火装置が必須である。この着火方法は特に規定されないが、より望ましいのは、熱風を温度制御して送風可能な電熱式ガスヒーター、電流量によって加熱温度をコントロール可能な電熱線の接触、および、電流量によって加熱温度をコントロール可能な赤外ランプによる着火である。熱を得るために燃料が必要な手法、例えばガスバーナーでは、燃料ガス及び排気ガスが、装置後段のガス検出器での検出に影響を及ぼすため、使用を避けるべきである。   Thirdly, the heating device portion of the sintering raw material will be described. The main heating method is an internal heating method by the combustion heat of the solid fuel embedded in the sintered raw material, and an ignition device for the solid fuel is essential. Although this ignition method is not particularly defined, it is more desirable to use an electric gas heater that can blow hot air by controlling the temperature of the hot air, contact of a heating wire that can control the heating temperature by the amount of current, and the heating temperature by the amount of current. Ignition by a controllable infrared lamp. In techniques that require fuel to obtain heat, such as a gas burner, the use of fuel gas and exhaust gas should affect the detection at the gas detector at the rear of the device and should be avoided.

以上の試料管部分、配管部分ならびに加熱装置部分にて試験を実施可能であるが、目的に応じて雰囲気ガス制御を行う場合には、反応管部分を容器4にて内包する。この反応雰囲気制御用容器の材質は耐熱性のガラス、石英等が、透明で装置内部を目視可能であり望ましい。   Although the test can be carried out in the above sample tube portion, piping portion and heating device portion, the reaction tube portion is enclosed in a container 4 when atmospheric gas control is performed according to the purpose. The reaction atmosphere control container is preferably made of heat-resistant glass, quartz or the like, which is transparent so that the inside of the apparatus can be visually observed.

第四に、装置の各所に接続する検出装置部分について説明する。焼結模擬試料に内装された固体燃料は炭素を主成分としており、その燃焼熱によって焼結模擬試料を加熱する。したがって、燃焼によって発生するCO、及びCO2の検出が必須であり、発明者らは赤外分光法を用いることで、簡便にかつ必要な測定が可能であることを確認している。また、燃焼条件である酸素分圧の制御や、ガス流速の制御のため、試料部分の温度測定を行う温度計、ガス流量計を設置する。また、試験の精度をより高めるため、配管の負圧計を設置することも有効である。 Fourthly, a description will be given of a detection device portion connected to each part of the device. The solid fuel contained in the sintered simulation sample is mainly composed of carbon, and the sintered simulation sample is heated by the combustion heat. Therefore, it is essential to detect CO and CO 2 generated by combustion, and the inventors have confirmed that simple and necessary measurement can be performed by using infrared spectroscopy. In addition, a thermometer and a gas flow meter for measuring the temperature of the sample portion are installed for controlling the oxygen partial pressure, which is a combustion condition, and for controlling the gas flow rate. It is also effective to install a negative pressure gauge for the piping in order to increase the accuracy of the test.

ガス流量計と負圧計は、配管のいずれの場所に設置することも可能であるが、焼結模擬試料の設置部の近くに配置することが望ましい。また、流量の変化について連続的に記録する装置を配置し、デジタル流量計とペンレコーダーやコンピューターの併用による記録を行う。   The gas flow meter and the negative pressure meter can be installed at any location of the piping, but it is desirable to arrange them near the installation portion of the sintered simulation sample. In addition, a device that continuously records changes in flow rate is arranged, and recording is performed by using a digital flow meter in combination with a pen recorder or a computer.

温度計については、焼結模擬試料の温度の測定が必須であり、その他、測定したい箇所に各々設置することも有効である。焼結模擬試料内部の温度測定には高温測定可能なR熱電対が有効である。また、サーモグラフィーによる観察も可能である。なお、温度の変化について連続的に記録する装置を配置し、ペンレコーダーやコンピューターを用いて記録を行う。   As for the thermometer, it is essential to measure the temperature of the sintered simulation sample, and it is also effective to install the thermometer at a place where it is desired to measure. An R thermocouple capable of high temperature measurement is effective for measuring the temperature inside the sintered simulation sample. Observation by thermography is also possible. A device that continuously records changes in temperature is arranged, and recording is performed using a pen recorder or a computer.

続いて、上記の焼結装置の使用方法について示す。
焼結試験装置の使用方法として、第一に、実験に供する焼結模擬試料(焼結原料と固体燃料の混合物)を予め混合し、試料管端部に設置する。第二に、ポンプによって試料管内部を吸引する。この時、ガス流量計によってガス流量を確認し、流量が規定の量になるようポンプもしくはバルブによって制御する。第三に加熱装置によって固体燃料に着火し、焼結模擬試料内部の温度計により、着火後の温度上昇を確認する。なお上記燃焼試験と同時に、燃焼により発生したCO、CO2を連続測定し記録するための操作を行う。
Subsequently, a method of using the above sintering apparatus will be described.
As a method of using the sintering test apparatus, first, a sintering simulation sample (a mixture of a sintering raw material and a solid fuel) to be used for the experiment is mixed in advance and placed at the end of the sample tube. Second, the inside of the sample tube is sucked by a pump. At this time, the gas flow rate is confirmed by a gas flow meter and controlled by a pump or a valve so that the flow rate becomes a specified amount. Thirdly, the solid fuel is ignited by the heating device, and the temperature rise after ignition is confirmed by the thermometer inside the sintered simulation sample. At the same time as the above combustion test, an operation for continuously measuring and recording CO and CO 2 generated by combustion is performed.

図2に本装置を用いた焼結試験によって得られたデータの一例を示す。   FIG. 2 shows an example of data obtained by a sintering test using this apparatus.

以上の使用方法によって、焼結模擬試験を実施可能であり、得られた燃焼時ガス発生のパターンと焼結試料を焼結鉱製造工程用の固体燃料の評価に用いる。   The sintering simulation test can be performed by the above method of use, and the obtained gas generation pattern during combustion and the sintered sample are used for evaluation of the solid fuel for the sinter manufacturing process.

上記の試験手順において所定のガス分析が可能である。本試験手順にて得られるガス分析結果の例を図2に示す。ガス分析器の読取からは、図2の上段の酸素分圧(濃度)の変化を示す実線のうちガス分析器の読み取りで酸素が検出されなくなったところ(図中のAで表示のところ)で、加熱装置によって焼結模擬試料を加熱する。この際、図2の実線で示される燃焼温度の変化を示す温度読み取り値について、所定の温度になる様に、加熱装置の出力制御を行う。続いて、燃焼開始後、曲線41、42、43で示されるようにCO2、CO、NO等の発生がガス分析器(FT−IR分析器)によって検出される。同時に、焼結模擬試料内の温度測定値が図2の下段の実線で示されるように読み取られ、各燃焼温度の燃焼時発生ガス濃度(分率)が検出可能となる。
また、ガス発生量を求める目的で、ガス流量の変動を測定する。その結果、図2の流量で示すような曲線を得られる。
Predetermined gas analysis is possible in the above test procedure. An example of a gas analysis result obtained by this test procedure is shown in FIG. From the reading of the gas analyzer, in the solid line showing the change in oxygen partial pressure (concentration) in the upper part of FIG. 2, when the gas analyzer no longer detects oxygen (indicated by A in the figure). The sintered simulation sample is heated by a heating device. At this time, the output control of the heating device is performed so that the temperature reading value indicating the change in the combustion temperature indicated by the solid line in FIG. 2 becomes a predetermined temperature. Subsequently, after the start of combustion, CO 2, CO as shown by the curve 41, the generation of NO or the like is detected by the gas analyzer (FT-IR analyzer). At the same time, the temperature measurement value in the sintered simulation sample is read as shown by the solid line in the lower part of FIG. 2, and the gas concentration (fraction) at the time of combustion at each combustion temperature can be detected.
In addition, the fluctuation of the gas flow rate is measured for the purpose of obtaining the gas generation amount. As a result, a curve as shown by the flow rate in FIG. 2 is obtained.

以下、上記のようにして得られた結果から、焼結鉱製造工程を評価する方法について説明する。   Hereinafter, a method for evaluating the sinter production process from the results obtained as described above will be described.

まず、焼結後の試料の歩留を求める。歩留の求め方は種々ある。例として、一般的な、焼結試料の強度を求める落下強度の測定や、焼結模擬試料の粒径より大きな目を持つふるいを使い塊化した試料の重量から求める方法や、焼結試料の光学顕微鏡観察から焼結試料同士の結合度を測る手法がある。発明者らは種々検討した中でも比較的少量の試料でも再現性よく歩留を求められる手法として、焼結模擬試験で得られた全試料のうち、原料粒度より大きくなった試料量S1と原料粒度以下の試料量S2よる次の式(1)
P=S1/(S1+S2) 式(1)
によって求められる塊率Pによって評価する手法が有効であることを確認した。ここで言う「原料粒度」とは、鉄鉱石原料の粒度を意味している。
First, the yield of the sintered sample is obtained. There are various ways to obtain the yield. For example, a general drop strength measurement for determining the strength of a sintered sample, a method for determining from the weight of a sample agglomerated using a sieve having a size larger than the particle size of the sintered simulated sample, There is a method of measuring the degree of bonding between sintered samples from observation with an optical microscope. As a method for obtaining a yield with a high reproducibility even in a relatively small amount of samples among the various inventors, among the samples obtained by the sintering simulation test, the sample amount S1 and the raw material particle size are larger than the raw material particle size. The following equation (1) with the following sample amount S2
P = S1 / (S1 + S2) Formula (1)
It was confirmed that the method of evaluating by the mass ratio P obtained by the above is effective. The “raw material particle size” here means the particle size of the iron ore raw material.

さらに、焼結鉱製造工程の生産速度を模擬した値として、焼結模擬試料の上面から下面までの燃焼の進行速度を求める。直接観察が可能な時には、実際に着火後下面まで火が広がる様を観察して速度を求められるが、加熱装置の構成や、試料面の直接観察が容易でないこともある。発明者らは、直接観察を不要とする手法として、焼結時発生ガス量の時間に対する変化を表すピークの半値幅Δt(s)と焼結模擬試料の充填高さh(mm)から、下記の式により焼結進行速度r(mm/s)を求めることも有効であることを確認した。
r=h(mm)/Δt(s) 式(2)
Furthermore, as a value simulating the production rate of the sintered ore production process, the progress speed of combustion from the upper surface to the lower surface of the sintered simulation sample is obtained. When direct observation is possible, the speed can be obtained by observing that the fire spreads to the lower surface after ignition, but the configuration of the heating device and the direct observation of the sample surface may not be easy. As a technique that eliminates the need for direct observation, the inventors have determined the following from the peak half-value width Δt (s) representing the change in the amount of gas generated during sintering over time and the filling height h (mm) of the sintered simulation sample. It was confirmed that it is also effective to obtain the sintering progress speed r (mm / s) by the following formula.
r = h (mm) / Δt (s) Equation (2)

半値幅の違いの例は図3の通りであり、同じ焼結模擬試料高さであっても、同図の(a)と(b)から明らかなように、試験の条件に応じてガス発生の半値幅は異なっており、結果的に得られる焼結進行速度rは異なる。   An example of the difference in half-value width is as shown in FIG. 3. Even if the sintered sample height is the same, as is clear from FIGS. The half-value widths of are different, and the resulting sintering progress rate r is different.

最終的に下式(3)にて、上記のPおよびrの積である焼結工程の評価値Svを求める。
Sv=P×r 式(3)
Finally, the evaluation value Sv of the sintering step, which is the product of P and r, is obtained by the following equation (3).
Sv = P × r Formula (3)

本発明者は、本発明による焼結模擬試験結果と従来技術による鍋試験結果との比較から、式(3)で与えられるSvが、鍋試験における生産率を予測するための指標として用い得ることを見出した。   The present inventor is able to use Sv given by the formula (3) as an index for predicting the production rate in the pan test from the comparison between the sintering simulation test result according to the present invention and the pan test result according to the prior art. I found.

本発明の焼結模擬試験による評価は焼結鉱製造工程における種々の条件、すなわち、鉱石原料の種類、焼結機の温度、風量等によって変化しうる。そのため、評価したい条件以外の条件を固定する。例えば、固体燃料を評価する場合は、鉱石原料、副原料等の種類、粒度、配合比等を一定とし、一定の温度、風量等の焼結条件で実験を行う。一方、固体燃料が決まった上で、最適な焼結条件を求める場合は、温度、風量等を変化させた試験を行う。   Evaluation by the sintering simulation test of the present invention can vary depending on various conditions in the sinter production process, that is, the type of ore raw material, the temperature of the sintering machine, the air volume, and the like. Therefore, the conditions other than the condition to be evaluated are fixed. For example, in the case of evaluating solid fuel, the experiment is performed under constant sintering conditions such as temperature and air flow, with the types of ore raw materials, auxiliary raw materials, etc., the particle size, the mixing ratio, etc. being constant. On the other hand, when the optimum sintering conditions are determined after the solid fuel is determined, a test with varying temperature, air volume, etc. is performed.

焼結鉱製造工程に用いる固体燃料の評価のため、原料鉄鉱石、焼結温度、ガス流量、酸素分圧を一定に制御し、固体燃料のみ変更した下記試験を行った。   In order to evaluate the solid fuel used in the sinter manufacturing process, the following tests were conducted in which the raw iron ore, sintering temperature, gas flow rate, and oxygen partial pressure were controlled to be constant and only the solid fuel was changed.

評価を行う固体燃料A〜Fについて、それぞれ、鍋試験と本発明による焼結模擬試験を行った。鍋試験の試料には、鉄鉱石84%、石灰16%をおよび固体燃料が外数で4%となるよう混合した焼結試料50kgを用い、試験装置に高さ600mmまで充填後、ブロアーで1500mmAqで大気を吸引しつつ、点火炉にて表層に90秒点火し焼成を行った。本発明による焼結模擬試験では、焼結模擬試料として、鍋試験と同等の同一銘柄の鉄鉱石84%、石灰16%の比率の混合物(焼結主原料)を800mg測りとり、上記混合物に粉状の固体燃料32mg(焼結主原料への添加量4%)を均一になるまで混ぜた後、水48mg(焼結主原料への添加量6%)で固めたものを用いた。   The solid fuels A to F to be evaluated were subjected to a pot test and a sintering simulation test according to the present invention, respectively. As a sample for the pan test, a sintered sample of 50 kg mixed with iron ore 84%, lime 16% and solid fuel so that the external number is 4% was used. After filling the test apparatus to a height of 600 mm, the blower was 1500 mmAq. Then, the surface layer was ignited for 90 seconds in an ignition furnace while the atmosphere was sucked, and firing was performed. In the sintering simulation test according to the present invention, 800 mg of a mixture (sintering main material) of the same brand of iron ore of 84% and lime of 16%, which is equivalent to the pot test, is measured as a sintering simulation sample, and the above mixture is powdered. The solid fuel 32 mg (addition amount 4% to the sintered main raw material) was mixed until uniform and then solidified with 48 mg water (addition amount 6% to the sintered main raw material).

焼結模擬試験の各条件は、所定の鍋試験の結果と比較するため、鍋試験の平均値を用い、温度は1400℃、ガス流量はガス流速が鍋試験と同等となるよう10L/min、酸素分圧は大気と同等、とした。   Each condition of the sintering simulation test is compared with the result of the predetermined pan test. The average value of the pan test is used, the temperature is 1400 ° C., the gas flow rate is 10 L / min so that the gas flow rate is equivalent to the pan test, The oxygen partial pressure was assumed to be equivalent to the atmosphere.

実験結果から得られた塊率P、焼結進行速度r、評価値Svと鍋試験の各固体燃料を用いた場合の生産率の結果を表1に示す。また、Svと生産率を比較したグラフを図4に示す。   Table 1 shows the results of the production rate when using the solid ratio P, the sintering progress rate r, the evaluation value Sv, and each solid fuel of the pot test obtained from the experimental results. Moreover, the graph which compared Sv and the production rate is shown in FIG.

Figure 0006372264
Figure 0006372264

その結果、Svが大きくなるにつれて鍋試験の生産率が良好となることが示された。同じ鍋試験装置を用い、同じ焼結試験条件において、標準的な固体燃料であるコークスを用いた場合の鍋試験の生産率は35t/d・m2であった。本生産率を閾値としたとき、Sv=8を超える焼結模擬試験評価値を示した固体燃料は、いずれも良好な鍋試験における生産率を示しており、焼結鉱製造工程に好適であると判断できた。 As a result, it was shown that the production rate of the pan test became better as Sv increased. The production rate of the pan test was 35 t / d · m 2 when coke as a standard solid fuel was used under the same sintering test conditions using the same pan test apparatus. When the production rate is set as a threshold value, the solid fuels showing the evaluation value of the sintering simulation test exceeding Sv = 8 all show the production rate in a good pot test and are suitable for the sinter manufacturing process. I was able to judge.

一方、本発明による焼結模擬試験で求められるSv値が高値の領域で鍋試験における生産率改善幅が縮小する理由は、加熱方法の違いによるものであり、外熱も用いる本発明の焼結模擬試験に対し、固体燃料の燃焼熱のみによって焼結する鍋試験では、燃焼温度が低くなるため、生産率が実機よりも低くなり、Sv値との乖離が生じていると考えられる。一方、本発明に用いられる焼結模擬試験における燃焼温度は、実機により近いので、Svは実機における生産率を予測するために用いることができると考えられる。   On the other hand, the reason why the production rate improvement width in the pan test is reduced in the region where the Sv value obtained in the sintering simulation test according to the present invention is high is due to the difference in the heating method, and the sintering of the present invention using external heat. In contrast to the simulation test, in the pot test in which sintering is performed only by the combustion heat of the solid fuel, the combustion temperature is low, so the production rate is lower than that of the actual machine, and it is considered that there is a deviation from the Sv value. On the other hand, since the combustion temperature in the sintering simulation test used in the present invention is closer to that of the actual machine, Sv can be used to predict the production rate in the actual machine.

1 試料(焼結原料)
2 試料保持部の端部
3 試料保持部の管
4 反応雰囲気制御用容器
1 Sample (Sintering raw material)
2 End of sample holder 3 Tube of sample holder 4 Container for reaction atmosphere control

Claims (2)

焼結鉱製造工程の評価方法であって、
〔1〕鉄鉱石原料と固体燃料とを含む0.01g以上10g以下の焼結模擬試料を用いた焼結模擬試験を、前記焼結模擬試料の表面温度をT(K)、焼結に必要な雰囲気ガスの単位時間あたりの送風量をV(m3/s)、前記雰囲気ガスの酸素分圧をPO2(kPa)、として、表面温度T、酸素分圧PO2、送風量Vを予め与えられた値に制御して行う工程と、
〔2〕前記焼結模擬試験時の前記固体燃料の燃焼ガスの測定を行う工程と、
〔3〕前記燃焼ガスの測定結果から燃焼速度を求める工程と、
〔4〕焼結試験後の焼結鉱試料の歩留を求める工程と、
〔5〕前記燃焼速度と前記歩留とから、前記焼結鉱製造工程を評価する工程、
とからなり、
工程〔2〕では、焼結時発生ガス量の時間に対する変化を表すピークの半値幅Δt(s)を求め、
工程〔3〕では、前記燃焼速度として、前記焼結模擬試料の充填高さh(mm)を工程〔2〕で求めた前記ピークの半値幅Δt(s)で除した、下記式(2)の焼結進行速度r(mm/s)を求め、
r=h(mm)/Δt(s) (2)
工程〔4〕では、焼結鉱試料の歩留を、前記焼結模擬試験で得られた全試料のうち、原料粒度より大きくなった試料量S1と原料粒度以下の試料量S2による次の式(1)
P=S1/(S1+S2) (1)
によって求められる塊率Pとして求め、
工程〔5〕では、以下の式(3)
Sv=P×r (3)
により焼結工程の評価値Svを求め、Sv=8を超える評価値を示した固体燃料を、焼結鉱製造工程に好適であると判断する、
ことを特徴とする焼結鉱製造工程の評価方法。
A method for evaluating a sinter production process,
[1] Sintering simulation test using 0.01 g or more and 10 g or less sintering simulated sample containing iron ore raw material and solid fuel, surface temperature of said sintered simulated sample is required for T (K), sintering A surface temperature T, an oxygen partial pressure PO2, and an air flow rate V are given in advance, where V (m 3 / s) is the air flow rate per unit time of the atmospheric gas, and oxygen partial pressure of the atmospheric gas is PO 2 (kPa). A process that is controlled to a specific value,
[2] a step of measuring the combustion gas of the solid fuel during the sintering simulation test;
[3] A step of obtaining a combustion rate from the measurement result of the combustion gas;
[4] A step of obtaining the yield of the sintered ore sample after the sintering test,
[5] A step of evaluating the sinter production process from the burning rate and the yield,
Ri Do not from the,
In the step [2], a half width Δt (s) of a peak representing a change with respect to time of the amount of gas generated during sintering is obtained,
In the step [3], as the burning rate, the filling height h (mm) of the sintered simulation sample is divided by the half-value width Δt (s) of the peak obtained in the step [2]. The sintering progress speed r (mm / s) of
r = h (mm) / Δt (s) (2)
In the step [4], the yield of the sintered ore sample is determined by the following equation based on the sample amount S1 larger than the raw material particle size and the sample amount S2 less than the raw material particle size among all the samples obtained in the sintering simulation test. (1)
P = S1 / (S1 + S2) (1)
Obtained as a mass ratio P obtained by
In step [5], the following formula (3)
Sv = P × r (3)
The evaluation value Sv of the sintering process is obtained by the above, and the solid fuel showing an evaluation value exceeding Sv = 8 is determined to be suitable for the sintered ore production process.
The evaluation method of the sintered ore manufacturing process characterized by the above-mentioned.
前記焼結模擬試料の量が0.5g以上1g以下であることを特徴とする、請求項1に記載の焼結鉱製造工程の評価方法。 The method for evaluating a sintered ore production process according to claim 1, wherein the amount of the sintered simulation sample is 0.5 g or more and 1 g or less.
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