JPS6020996A - Plant for coal liquefaction or production of regenerated coal - Google Patents
Plant for coal liquefaction or production of regenerated coalInfo
- Publication number
- JPS6020996A JPS6020996A JP12834583A JP12834583A JPS6020996A JP S6020996 A JPS6020996 A JP S6020996A JP 12834583 A JP12834583 A JP 12834583A JP 12834583 A JP12834583 A JP 12834583A JP S6020996 A JPS6020996 A JP S6020996A
- Authority
- JP
- Japan
- Prior art keywords
- coal
- steel
- temperature
- containers
- plant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
Description
【発明の詳細な説明】
この発明は石炭液化プラントもしくは石炭液化技術を応
用した一生炭製造プラントに開広特にそのプラントに使
用される容器材料に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a coal liquefaction plant or a coal production plant applying coal liquefaction technology, and particularly to a container material used in such a plant.
周知のように石炭の液化技術は第２医大戦前から石油資
源の乏しい国において開発が進められていたが、その当
時は実用化に至らず、第２次大戦後は安価な石油が入手
容易となったため石炭液化の開発研究は下火となってい
た。しかしながら近年は原油価格の高騰と石油資源自体
の量的制限等から、石炭が見直され、その液化技術の実
用化のための研究開発が再び盛んに行なわれるようにな
っている。また一方、石炭資源それ自体は未だ豊富とは
いえども、製鉄用コークスの原料となシ得る良質な粘結
炭は量的に制限されるから、最近では石炭液化技術を応
用して、従来は製鉄用コークスの原料炭とはなり得なか
った一般炭を改質し、その改質されたいわゆる再生炭を
製鉄用コークスの原料として利用する技術が脚光を浴び
ている。As is well known, coal liquefaction technology had been under development in countries with poor oil resources since before the Second Medical War, but it had not been put to practical use at that time, and after World War II cheap oil became easier to obtain. As a result, research into the development of coal liquefaction has slowed down. However, in recent years, coal has been reconsidered due to soaring crude oil prices and quantitative limitations on petroleum resources themselves, and research and development for the practical application of coal liquefaction technology has once again become active. On the other hand, although coal resources themselves are still abundant, the quantity of high-quality coking coal that can be used as a raw material for steelmaking coke is limited, so recently coal liquefaction technology has been applied to BACKGROUND ART A technology in which steam coal, which could not be used as coking coal for steelmaking coke, is reformed and the reformed so-called recycled coal is used as a raw material for steelmaking coke is attracting attention.
ところで上述のような石炭液化プラントや再生炭製造プ
ラントにおいては、石炭の分解液イし反に６が起る反応
塔、あるいは石炭の分解液化反応で生じた種々の物質を
分離精製するだめの分離塔など、多数の容器が用いられ
ている。石炭液化反応に伴って生成される化学種として
は、水素と、石炭中の炭素、酸素、窒素、硫黄、塩素と
の反応によって生じるｃｏ 、 ｃｏ２． ｕ２ｏ 、
ａ２ｓ 、 ＣＨ４，ＮＨ３゜ＨＣＮ 、 ＨＣｌな
ど種々多様なものかあ）、これらの液化反応生成物質が
容器材料の腐食因子となり、高温高圧下であることも加
わって、複雑かつＵ酷の問題は極めて重要であり、上述
のように複雑力）つ苛酷な腐食環境に耐え得る容器材料
の選定力五石炭液化、再生炭製造技術の実用化の成否を
握っているといっても過言ではない。しかるに石炭液化
、再生炭製造プラント容器材料についての開発・研究は
未だ不充分であり、現段階では従来の池の化学プラント
等から得た経験に基いて石炭液化プラント、再生炭製造
プラントの容器材料を選定しているに過ぎず、これらの
プラント容器材料に真に最適な材料、すなわちこれらの
プラントに個有の腐食環境における耐食性、耐高温１液
化性、あるいは経済性等の面から真に適切な材料が選定
されているとは言い難いのが実情である。By the way, in the above-mentioned coal liquefaction plants and recycled coal manufacturing plants, there is a reaction tower where 6 occurs in the coal decomposition liquid, or a separation tank where various substances produced in the coal decomposition and liquefaction reaction are separated and purified. A number of containers are used, including towers. Chemical species generated in the coal liquefaction reaction include co, co2. u2o,
A2s, CH4, NH3゜HCN, HCl, etc.), these liquefaction reaction product substances become corrosive factors for container materials, and when combined with the high temperature and high pressure conditions, the problem becomes extremely complex and severe. It is no exaggeration to say that the success or failure of the practical application of coal liquefaction and recycled coal manufacturing technology will be determined by the importance of selecting container materials that can withstand the harsh corrosive environment. However, development and research on container materials for coal liquefaction plants and recycled coal manufacturing plants is still insufficient, and at this stage, based on the experience gained from conventional pond chemical plants, etc., container materials for coal liquefaction plants and recycled coal manufacturing plants are being developed. We only select materials that are truly optimal for these plant containers, that is, materials that are truly appropriate in terms of corrosion resistance in the corrosive environment unique to these plants, high-temperature single-liquid resistance, or economic efficiency. The reality is that it is difficult to say that the most suitable materials have been selected.
この発明は以上の事情に鑑みてなされたもので、石炭液
化もしくは再生炭製造プラントの容器としての個有の腐
食環境に対して安全な、高い耐食性および耐酸化性を有
し、しかも経済性にも優れた材料を用いた容器で構成し
た石炭液化もしくは再生炭製造プラントを提供すること
を目的とするものであυ、特にそのプラント運転中に曝
される個々の容器温度に応じて安全性、経済性の両面か
ら最適な容器材料を選定したプラントを提供するもので
ある。This invention was made in view of the above circumstances, and has high corrosion resistance and oxidation resistance that is safe against the corrosive environment unique to coal liquefaction or recycled coal production plant containers, and is also economically efficient. The purpose of this project is to provide a coal liquefaction or recycled coal manufacturing plant constructed with containers made of superior materials, with particular safety and This provides a plant in which the optimal container material is selected from both economical and economical perspectives.
すなわち本発明者等は、石炭液化もしくは再生炭製造プ
ラントの容器材料としてＣ，ｒおよび／またはＭｏを含
有する鋼を選択することとし、再生炭製造プラントの各
種容器中でＣｒ ｆ Ｍｏ量の異なる各種の鋼材につい
て実際の運転環境下で曝露試験を行ったところ、鋼材の
Ｃｒ 十Ｍｏ量によって使用可能な限界の温度があり、
運転中に曝され、る容器内温度に応じて、安全性と経済
性との兼ね合いから適切なＣｒ −Ｆ Ｍｏ量があるこ
とを見出し、この発明をなすに至った。That is, the present inventors decided to select steel containing C, r, and/or Mo as a container material for a coal liquefaction or recycled coal production plant, and that steel with different amounts of Cr f Mo was selected in various containers of the recycled coal production plant. When we conducted exposure tests on various steel materials under actual operating environments, we found that there is a limit temperature at which the steel can be used, depending on the amount of Cr and Mo.
The inventors have discovered that there is an appropriate amount of Cr-F Mo depending on the temperature inside the container to which it is exposed during operation, taking into account the balance between safety and economic efficiency, leading to the creation of this invention.
具体的には、この発明の石炭液化もしくは再生炭製造プ
ラントは、少くとも内面がＣ「および／またはＭｏを含
有する鋼材で形成された複数の容器を備えてなシ、かつ
それらの容器のうち、運転中に曝される温度が１００℃
以下の容器についてはＣｒおよび／またはＭｏの合計含
有量が６チ以°ドの銅材を、１００〜２００℃の容器に
ついてはＣｒおよび／またはＭｏの合計含有量が６チを
越え１４チ以下の銅材を、２００〜４００℃の容器につ
いてはＣｒおよび／またはＭｏの合計含有量が１４チを
越え２０チ以下の鋼材を、４００℃以上の容器について
はＣｒおよび／またはＭｏの合計含有量が２０チを越え
る鋼材を用いていることを特徴とするものである。Specifically, the coal liquefaction or recycled coal production plant of the present invention does not include a plurality of containers whose inner surfaces are made of a steel material containing at least C and/or Mo, and , the temperature exposed during operation is 100℃
For the following containers, use copper material with a total content of Cr and/or Mo of 6 cm or more; for containers at 100 to 200°C, use copper material with a total content of Cr and/or Mo of more than 6 cm and 14 cm or less. For containers with a temperature of 200 to 400℃, use steel materials with a total content of Cr and/or Mo exceeding 14 inches and 20 inches or less, and for containers with a temperature of 400℃ or higher, a total content of Cr and/or Mo. It is characterized by using steel material with a diameter exceeding 20 inches.
以下この発明についてさらに詳細に説明する。This invention will be explained in more detail below.
石炭液化の方法には、大別して水添液化法、溶剤抽出法
、乾留法、合成液化法などがあるが、これらのうち水添
加法は再生炭製造プラントとほぼ同じプロセスである。Coal liquefaction methods can be broadly classified into hydrogen liquefaction methods, solvent extraction methods, carbonization methods, and synthetic liquefaction methods, among which the water addition method is almost the same process as in recycled coal manufacturing plants.
この再生炭製造プラントの一例を第１図に示す。この再
生炭製造プラントは製鉄用コークスの原料とはなシ得な
いような一般炭を原料とし、これを改質して製鉄用コー
クスの原料となシ得る再生炭を得ることを主目的としだ
ものであるが、このプラントでも再生炭の製造と同時に
、軽質油、重質油等の石炭を液化した油分が得られる。An example of this recycled coal manufacturing plant is shown in Figure 1. The main purpose of this recycled coal manufacturing plant is to use steam coal, which cannot be used as a raw material for coke for steel manufacturing, as a raw material, and to reform it to obtain recycled coal that can be used as a raw material for coke for steel manufacturing. However, at the same time as producing recycled coal, this plant also produces oil components such as light oil and heavy oil that are obtained by liquefying coal.
そして石炭液化を主目的とする場合は、第１図のプロセ
ス中の反応塔１内における反応の程度を高めれば良く、
その他は実質的に第１図に示されるものと同じプロセス
で良い。If coal liquefaction is the main purpose, it is sufficient to increase the degree of reaction in the reaction tower 1 during the process shown in Figure 1.
Otherwise, the process may be substantially the same as that shown in FIG.
本発明者等は、第１図に示されるような再生炭製造プラ
ントにおいて、異なる腐食環境に罎されるいくつかの容
器内、例えば反応塔１、分離塔２゜３、吸収塔４、減圧
ドラム５などの内面に、ｃｒおよび／またはＭｏを含有
しかつＣｒ 十Ｍｏ 最の異なる種々の鋼材を曝露させ
て実際のプラント運転中の腐食環境に曝す試験を２回に
わたって実施し、各鋼材の腐食速度を調査した。そして
、容器内温度を腐食因子としてとシあげて、温度が各鋼
材の腐食速度に及ぼす影響を整理したところ、第２図に
示す結果が得られた。但し第２図において各部（○、・
、−△、ム）は、図中に記した各Ｃ’ｒ ＋ Ｍ。In a regenerated coal production plant as shown in FIG. A test was carried out twice in which various steel materials containing Cr and/or Mo containing Cr and/or Mo were exposed to the corrosive environment during actual plant operation, and the corrosion of each steel material was I checked the speed. Then, by considering the temperature inside the container as a corrosion factor and arranging the influence of temperature on the corrosion rate of each steel material, the results shown in FIG. 2 were obtained. However, in Figure 2, each part (○,・
, -△, M) are each C'r + M written in the figure.
量範囲に入る４〜６鋼種の１回の曝露試験における腐食
速度の平均値を示す。It shows the average value of the corrosion rate in one exposure test of 4 to 6 steel types falling within the weight range.
上述の腐食試験においては、温度以外の贋食因子は容器
ごとに異なるにもかかわらず、第２図から明らかなよう
に腐食速度は温度と強い相関関係があり、鋼中のＣｒ
＋ Ｍｏ量で定まるある臨界温度を越えれば、温度の上
昇とともに腐食速度は約０、１ ｒＨｊ／ｙｅａｒを越
えて急激に大きくなる。この臨界温度は、Ｃｒ ＋ Ｍ
ｏ量が６チ以下の鋼においては１００℃、６％（Ｃｒ
＋ Ｍｏ≦１４俤の鋼においては２００℃、１４ ＜
Ｃｒ ＋ Ｍｏ≦２０％の鋼においては３００℃、Ｃｒ
＋ Ｍｏ ＞ ２０ ％の鋼においては４５０℃以上
となる。通常の実操業においては、腐食速度が約０．１
１１％”ｙｅａｒ以Ｆが安全性等の点からＣｒ ＋ Ｍ
ｏ量の銅はそれぞれの上記臨界温度以Ｆで使用すること
が安全性の点から必要であることがわかる。一方、経済
性の点からは、Ｃｒ 、 Ｍｏは高価であるから、可及
的にＣｒ ｆ Ｍｏ量の少ない鋼材を使用することが好
ましい。したがって経済性と安全性との兼ね合いから、
再生炭製造プラントあるいは水添加法による石炭液化プ
ラントの容器材料としては、
１００℃以下の容器にはＣｒ十Ｍｏ≦６俤の鋼材、１０
０〜２００℃の容器には６ 〈、Ｃｒ 、＋ Ｍｏ≦１
４Ｌｌ）の鋼材、２００〜４００℃の容器には１４ ＜
Ｃｒ ＋Ｍｏ≦２０％のＸ材、
４００℃以上の容器にはＣｒ 十Ｍｏ ＞ ２０ ％の
鋼材をそれぞれ使用することが、最も経済的でしかも腐
食に対して安全であることがわかる。In the above-mentioned corrosion test, although corrosion factors other than temperature differ depending on the container, as is clear from Figure 2, the corrosion rate has a strong correlation with temperature, and Cr in steel
+ Once a certain critical temperature determined by the amount of Mo is exceeded, the corrosion rate rapidly increases to exceed about 0.1 rHj/year as the temperature rises. This critical temperature is Cr + M
For steels with an o content of 6 or less, 100°C and 6% (Cr
+ For steel with Mo≦14, 200℃, 14<
For steel with Cr + Mo≦20%, at 300°C, Cr
+Mo > 20% steel has a temperature of 450°C or higher. In normal actual operation, the corrosion rate is approximately 0.1
11%"year and above F is Cr+M from the point of view of safety etc.
It can be seen that it is necessary from the viewpoint of safety to use the amount of copper at a temperature below the above-mentioned critical temperature. On the other hand, from an economic point of view, since Cr and Mo are expensive, it is preferable to use a steel material with as little Cr f Mo as possible. Therefore, from a balance between economy and safety,
Container materials for recycled coal production plants or coal liquefaction plants using the water addition method include steel materials with Cr10Mo≦6 tons, and 10
6〈, Cr, + Mo≦1 for the container at 0 to 200℃
4Ll) steel material, 14< for containers at 200-400℃
It can be seen that it is the most economical and safe against corrosion to use the X material with Cr + Mo ≦ 20% and the steel material with Cr + Mo > 20% for containers at 400° C. or higher.
以上のように、石炭液化プロセスとほぼ同じ実際の再生
炭製造プラントにおいて腐食実験を行い、かつその実験
結果を温度とＣｒ ＋ Ｍｏ量に関して体系的に整理す
ることによシ、それらのプラントの容器材料の鋼材とし
て、温度に応じて経済性と腐食に対する安全性との両者
を満足する最適なＣｒ＋Ｍｏ含有量があることを本発明
者が初めて見出し、この発明を完成させたのである。As described above, by conducting corrosion experiments in actual recycled coal manufacturing plants that are almost the same as those in the coal liquefaction process, and systematically organizing the experimental results in terms of temperature and Cr + Mo content, it was possible to The present inventor was the first to discover that there is an optimal Cr+Mo content for the steel material that satisfies both economic efficiency and corrosion safety depending on the temperature, and has completed this invention.
なお石炭液化もしくは再生炭製造プラントに使用される
各種容器のうち、特に蒸留塔（フラクショネータ）につ
いては、その温度が下部で３００℃、中部および上部で
２００ ’Ｃ程度であるにもかかわらず、塔内で気化液
化を繰返し、不純物の濃縮が起るなど、極めて厳しい腐
食環境となってお１） 、Ｃｒ 十Ｍｏ ｔｔが２０チ
以上のステンレス鋼でも腐食速度は２０ ＭＰＹ （０
，５ｍｒｒｙ’ｙｅａｒ ） 〜２０００ＭＰＹ （５
０ｍｉｎ／ｙｅａｒ ）に達し、したがって前記の温度
による材料選定基準から蒸留塔は除くべきであり、通常
は蒸留塔用の容器材料としてはＦｅ基以外の金属、例え
ばＴｉやハステロイＣ−２７６などを使用することが望
ましい。Among the various containers used in coal liquefaction or recycled coal production plants, the temperature of distillation columns (fractionators) in particular is 300°C at the bottom and about 200°C at the middle and upper parts. , repeating vaporization and liquefaction in the column causes concentration of impurities, creating an extremely harsh corrosive environment.1) Even for stainless steel with a Cr+Mott of 20 or more, the corrosion rate is 20 MPY (0
,5mrry'year) ~2000MPY (5
Therefore, distillation columns should be excluded from the material selection criteria based on temperature mentioned above, and metals other than Fe-based, such as Ti and Hastelloy C-276, are usually used as container materials for distillation columns. It is desirable to do so.
なおまた、前記の温度によるＣｒ ＋ Ｍｏ量の規定は
、ＣｒもしくはＭｏの一方のみを含有する場合も有効で
あり、その場合その単独量が前記範囲を満足すれば良い
。またこの発明においては鋼材中のＣｒ 、 Ｍｏ以外
については特に規定しないが、ＣｒやＭＯのほか、溶接
性や靭性の改善のためＮｉを６〜２０チ程度含有させた
り、壕だ溶接熱影響部の靭性改善のためにＮｂを０．０
１〜０４チ程度含有させた鋼材でも良い。さらに、前記
の規定によるＣｒおよび／まだはＭｏを含有する鋼材は
、通常の圧延−熱処理材で充分であシ、またその鋼材は
少くとも容器内面に形成されていれば良く、シたがって
他の構造材からなる容器本体の内面にｔＭｌ記の規定に
よる鋼材を内張すしても、あるいは容器全体を前記の規
定による鋼材で形成しても良い。Furthermore, the above-mentioned regulation of the amount of Cr + Mo based on the temperature is also effective when only one of Cr or Mo is contained, and in that case, it is sufficient that the single amount thereof satisfies the above range. In addition, in this invention, other than Cr and Mo in the steel material are not particularly stipulated, but in addition to Cr and MO, about 6 to 20 Ni may be included to improve weldability and toughness, and trench welding heat affected zone may be added. Adding 0.0 Nb to improve the toughness of
A steel material containing approximately 1 to 0.04% may also be used. Further, as the steel material containing Cr and/or Mo according to the above regulations, it is sufficient to use ordinary rolling and heat treatment material, and it is sufficient that the steel material is formed at least on the inner surface of the container. The inner surface of the container body made of the structural material may be lined with a steel material according to the regulations specified in tMl, or the entire container may be formed from a steel material according to the regulations specified above.
次に、実際の再生炭製造プラントの容器として各種鋼材
を使用した実施列を第１表に示す。第１表において、容
器４１．．４６２はこの発明を満足する鋼材で作られた
もの、また容器ｙｆ６３．／１６４はこの発明で規定す
る範囲を外れる鋼材で作られたものであシ、ご丸らにつ
いて１年間使用後の厚みの減少量を１容器につき１０ケ
所測定し、その平均値をめた。Next, Table 1 shows examples of cases in which various steel materials were used as containers in actual recycled coal manufacturing plants. In Table 1, container 41. ．． 462 is made of steel that satisfies this invention, and container yf63. /164 was made from a steel material outside the range specified by this invention.The amount of decrease in thickness of Gomaru et al. after one year of use was measured at 10 locations per container, and the average value was calculated.
第１表
第１表に示すように、この発明で規定する範囲を満足す
る／１６１．／Ｉ６２の容器は肉厚の減少量が０．１日
未満と著しく小さいのに対し、この発明で規定する範囲
を外れる１６３．痛４の容器は肉厚減少量が０．５〜０
．８囚と極めて大きかった。Table 1 As shown in Table 1, /161. The amount of decrease in wall thickness of the container of /I62 is extremely small at less than 0.1 day, whereas the amount of decrease in wall thickness of the container of 163. Ita 4 containers have a wall thickness reduction of 0.5 to 0.
．． It was extremely large with 8 prisoners.
以上のようにこの発明の石炭液化もしくは再生炭、製造
プラントは、容器温度に応じてその容器材料としての鋼
材のＣｒ ＋ Ｍｏ含有量を適切に選ぶことによって、
経済性と腐食に対する安全性との両者を同時に満足させ
得る顕著な効果を有するものである。As described above, the coal liquefaction or recycled coal production plant of the present invention can achieve
This has the remarkable effect of satisfying both economic efficiency and safety against corrosion at the same time.
第１図は再生炭製造プラントの一例を示すフローチャー
ト、第２図は再生炭製造プラントにおける容器温度と腐
食速度との関係を、Ｃｒ＋Ｍｏ量をパラメータとして表
わす相関図である。
出願人 川崎製鉄株式会社
代理人 弁理士豊田武人
（ほか１名）FIG. 1 is a flowchart showing an example of a recycled coal manufacturing plant, and FIG. 2 is a correlation diagram showing the relationship between container temperature and corrosion rate in the recycled coal manufacturing plant using the amount of Cr+Mo as a parameter. Applicant: Kawasaki Steel Co., Ltd. Agent: Taketo Toyota, patent attorney (and one other person)
Claims (1)
で形成された複数の容器を備えてなシ、かつそれらの容
器のうち、運転中に曝される温度が１００℃以下の容器
については前記鋼材としてＣｒおよび／またはＭｏの合
計含有量が６チ（重量％、以下同じ）以下のものを、１
００〜２００℃の容器については前記鋼材としてＯｒお
よび／またはＭｏの合計含有量が６チを越え１４％以下
のものを、２００〜４００℃の容器については前記鋼材
としてＣｒおよび／またはＭｏの合計含有量が１４％を
越え２０チ以下のものを、４００℃以上の容器について
は前記鋼材としてＣｒおよび／またはＭｏの合計含有量
が２０チを越えるものをそれぞれ用いていることを特徴
とする石炭液化もしくは再生炭製造プラント。It must be equipped with a plurality of containers whose inner surfaces are made of a steel material containing at least Cr and/or Mo, and among these containers, containers to which the temperature to which they are exposed during operation is 100°C or less are made of the above-mentioned steel material. The total content of Cr and/or Mo is 6% or less (weight%, same below) as 1
For containers with a temperature of 00 to 200°C, the steel material should have a total content of Or and/or Mo exceeding 6% and not more than 14%, and for containers with a temperature of 200 to 400°C, the steel material should have a total content of Cr and/or Mo. Coal having a total Cr and/or Mo content of more than 14% and 20% or less is used as the steel material, and for containers with a temperature of 400°C or higher, a steel with a total content of Cr and/or Mo exceeding 20% is used. Liquefied or recycled coal production plants.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12834583A JPS6020996A (en) | 1983-07-14 | 1983-07-14 | Plant for coal liquefaction or production of regenerated coal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12834583A JPS6020996A (en) | 1983-07-14 | 1983-07-14 | Plant for coal liquefaction or production of regenerated coal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6020996A true JPS6020996A (en) | 1985-02-02 |
Family
ID=14982508
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12834583A Pending JPS6020996A (en) | 1983-07-14 | 1983-07-14 | Plant for coal liquefaction or production of regenerated coal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6020996A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4861441A (en) * | 1986-08-18 | 1989-08-29 | Nippon Steel Corporation | Method of making a black surface treated steel sheet |
-
1983
- 1983-07-14 JP JP12834583A patent/JPS6020996A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4861441A (en) * | 1986-08-18 | 1989-08-29 | Nippon Steel Corporation | Method of making a black surface treated steel sheet |
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