JP2556142B2 - lubricant - Google Patents
lubricantInfo
- Publication number
- JP2556142B2 JP2556142B2 JP1228975A JP22897589A JP2556142B2 JP 2556142 B2 JP2556142 B2 JP 2556142B2 JP 1228975 A JP1228975 A JP 1228975A JP 22897589 A JP22897589 A JP 22897589A JP 2556142 B2 JP2556142 B2 JP 2556142B2
- Authority
- JP
- Japan
- Prior art keywords
- lubricant
- present
- guide shoe
- aggregate
- pickling
- 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.)
- Expired - Lifetime
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B45/00—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills
- B21B45/02—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills for lubricating, cooling, or cleaning
- B21B45/0239—Lubricating
- B21B45/0242—Lubricants
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B25/00—Mandrels for metal tube rolling mills, e.g. mandrels of the types used in the methods covered by group B21B17/00; Accessories or auxiliary means therefor ; Construction of, or alloys for, mandrels or plugs
- B21B25/04—Cooling or lubricating mandrels during operation
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Lubricants (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は、たとえば熱間管圧延におけるガイドシュー
疵の発生を防止するのに好適な潤滑剤に関する。TECHNICAL FIELD The present invention relates to a lubricant suitable for preventing the occurrence of guide shoe defects in, for example, hot pipe rolling.
（従来の技術） 潤滑剤は、熱間管圧延、特にマンネスマン方式の熱間
管圧延の際に必要であり、ガイドロールとの接触部分に
おける、製品のガイドシュー疵の発生を防止する効果を
有する。(Prior Art) Lubricant is necessary for hot tube rolling, especially Mannesmann hot tube rolling, and has an effect of preventing the occurrence of guide shoe flaws of the product at the contact portion with the guide roll. .
このような潤滑剤としては、特開昭61−223096号公報
により提案されているように、潤滑剤の主成分として酸
化鉄を用いるケースも増えてきた。As such a lubricant, there is an increasing number of cases where iron oxide is used as the main component of the lubricant, as proposed by JP-A-61-223096.
（発明が解決しようとする課題］ しかし、この特開昭61−223096号公報により提案され
た手段は、酸化鉄、ケイ酸化合物およびアルキレン重合
体を必要とするためにコスト的に不利であるとともに、
潤滑剤としての効果、すなわち熱間管圧延の際のガイド
シュー疵の発生防止効果が少ないという問題があった。(Problems to be Solved by the Invention) However, the means proposed by JP-A-61-223096 is disadvantageous in cost because it requires iron oxide, a silicic acid compound and an alkylene polymer. ,
There is a problem that the effect as a lubricant, that is, the effect of preventing the generation of guide shoe defects during hot tube rolling is small.
すなわち、従来の手段では、たとえば熱間管圧延にお
けるガイドシュー疵の発生を防止するのに好適な潤滑剤
を安価に得ることばできなかったのである。That is, with the conventional means, it was not possible to inexpensively obtain a lubricant suitable for preventing the occurrence of guide shoe flaws in, for example, hot pipe rolling.
ここに、本発明の目的は上記の課題を解決することは
可能な潤滑剤を提供することにある。An object of the present invention is to provide a lubricant capable of solving the above problems.
（課題を解決するための手段） 本発明者らは上記の課題を解決するため、種々検討を
重ねた結果、鉄鋼を酸洗した後の酸洗廃液を原料として
磁性酸化鉄を製造すれば廉価な磁性酸化鉄が得られ、こ
れを潤滑剤として用いることができることを知見した。(Means for Solving the Problems) The inventors of the present invention have conducted various studies to solve the above problems, and as a result, it is inexpensive to produce magnetic iron oxide using the pickling waste liquid after the pickling of steel as a raw material. It has been found that a magnetic iron oxide having various properties can be obtained and can be used as a lubricant.
しかし、鉄鋼を酸洗した後の酸洗廃液から得た磁性酸
化鉄（Fe3O4、以下同じ）は微粉であるため、このまま
潤滑剤として用いたのでは、得られる潤滑剤の強度が低
く、潤滑剤として求められる耐久性が不足するという問
題があった。However, magnetic iron oxide (Fe 3 O 4 , the same hereafter) obtained from pickling waste liquid after pickling steel is fine powder, so if it is used as a lubricant as it is, the strength of the obtained lubricant is low. However, there is a problem that the durability required as a lubricant is insufficient.
そこで、本発明者らは、さらに検討を重ねた結果、鉄
鋼を酸洗した後の酸洗廃液から得られる磁性酸化鉄に、
耐火性向上を目的として耐火性向上成分および粘着成分
を混練することにより、たとえば熱間管圧延におけるガ
イドシュー疵の発生を防止するのに好適な潤滑剤を得る
ことが可能であることを知見した。Therefore, as a result of further studies, the present inventors have found that in a magnetic iron oxide obtained from a pickling waste liquid after pickling steel,
It has been found that it is possible to obtain a lubricant suitable for preventing the occurrence of guide shoe flaws, for example, in hot tube rolling by kneading the fire resistance improving component and the adhesive component for the purpose of improving fire resistance. .
また、この磁性酸化鉄から得られる潤滑剤を用いる際
には、例えば鉱石から粉石して得られる骨材をある適当
な量配合して潤滑剤の強度を増すことも有効であること
を知見して、本発明を完成した。Further, when using a lubricant obtained from this magnetic iron oxide, it was found that it is also effective to increase the strength of the lubricant by, for example, compounding an appropriate amount of aggregate obtained by powdering ore. Then, the present invention was completed.
ここに、本発明の要旨とするところは、鉄鋼を酸洗し
た後の酸洗廃液から得た磁性酸化鉄と耐火成分と粘結剤
と水とを混練してなる潤滑剤である。Here, the gist of the present invention is a lubricant obtained by kneading magnetic iron oxide, a refractory component, a binder, and water obtained from a pickling waste liquid after pickling steel.
また、別の面からは、本発明は、上記の潤滑剤と骨材
とを1:3〜５の重量割合で混練してなる潤滑剤である。From another aspect, the present invention is a lubricant obtained by kneading the above-mentioned lubricant and aggregate in a weight ratio of 1: 3 to 5.
なお、本発明において、「骨材」とは、例えば鉱石か
ら砕石したものであって、その粒径は後述するように50
〜200μｍ程度が望ましい。また、骨材の原料として
は、鉄鉱石、特にＳ、Ｐ等の不純物が少なく、鉄分の多
い良質な鉄鉱石が好ましい。In the present invention, the “aggregate” is, for example, crushed stone from ore, and its particle size is 50 as described later.
Approximately 200 μm is desirable. Further, as a raw material of the aggregate, iron ore, particularly high-quality iron ore containing few impurities such as S and P and having a large iron content is preferable.
（作用） 以下、本発明を作用効果とともに詳述する。なお、本
明細書において、「％」は特にことわりがない限り、
「重量％」を意味するものとする。(Operation) Hereinafter, the present invention will be described in detail together with operation effects. In addition, in the present specification, “%” is, unless otherwise specified,
It means "% by weight".
まず、鉄鋼を酸洗した後の酸洗廃液、たとえば塩酸廃
液には、FeCl2等の塩化鉄が含まれている。この塩化鉄
から磁性酸化鉄（Fe3O4）を生成させるため、たとえ
ば、まず酸洗廃液にMgO、Ca（OH）２またはNaOH等のア
ルカリ、またはアルカリ土類金属の酸化物または水酸化
物、空気、さらには必要に応じて高温蒸気を加える。こ
のときの反応は、たとえば FeCl2＋Ca（OH）２→Fe（OH）２＋CaCl2 3Fe（OH）２＋1/202→Fe3O4↓＋3H2O となる。First, a pickling waste liquid after pickling steel, such as a hydrochloric acid waste liquid, contains iron chloride such as FeCl 2 . In order to produce magnetic iron oxide (Fe 3 O 4 ) from this iron chloride, for example, first, the pickling waste liquid is an alkali or alkaline earth metal oxide or hydroxide such as MgO, Ca (OH) 2 or NaOH. , Add air, and optionally high temperature steam. The reaction at this time is, for example, FeCl 2 + Ca (OH) 2 → Fe (OH) 2 + CaCl 2 3Fe (OH) 2 +1/20 2 → Fe 3 O 4 ↓ + 3H 2 O.
上記の反応を促進するために、前述したように必要に
応じて、温度の上昇を促進させる目的で高温蒸気を加え
ることが有効である。In order to promote the above reaction, it is effective to add high temperature steam for the purpose of accelerating the temperature rise as described above.
このようにして生成したFe3O4の沈澱を脱水・分離に
より回収した後、沈澱物を水洗浄し、再び脱水・分離し
た後、少量の水を加えて、Fe3O4スラリーとした後、た
とえばAl2O3、SiO2、MgO等の耐火性向上成分（耐火成
分）を加えて熱間での耐用性を向上させる。The Fe 3 O 4 precipitate thus formed was recovered by dehydration / separation, washed with water, dehydrated / separated again, and a small amount of water was added to form a Fe 3 O 4 slurry. For example, a fire resistance improving component (refractory component) such as Al 2 O 3 , SiO 2 and MgO is added to improve hot durability.
さらに、Na2SiO3（水ガラス）などの粘結剤と追加水
を加え、混練する。水の量は潤滑剤として適当な粘度を
得るように調整する。粘度は、4,000〜10,000cps程度が
作業性等の観点から好適である。粘結剤としては、MgO
等がさらに例示される。ここで、MgOは前述したような
耐火性向上成分の他に、粘結剤としても作用する。Further, a binder such as Na 2 SiO 3 (water glass) and additional water are added and kneaded. The amount of water is adjusted to obtain an appropriate viscosity as a lubricant. A viscosity of about 4,000 to 10,000 cps is suitable from the viewpoint of workability and the like. MgO as a binder
Etc. are further exemplified. Here, MgO also acts as a binder in addition to the above-mentioned fire resistance improving component.
なお、各成分の配合量としては、たとえば Fe3O4:10〜30％ Al2O3:5〜15％ SiO2:15〜30％ Na2SiO3:15〜25％ MgO:5〜10％ K2B:0.1〜0.2％ が例示される。この結果は、第１表に示す実験結果に基
づくものである。なお、第１表に示す試験項目の中で
は、本発明においては、耐火度、高温剥離性および潤滑
性が特に重要である。As the amount of each component, for example, Fe 3 O 4: 10~30% Al 2 O 3: 5~15% SiO 2: 15~30% Na 2 SiO 3: 15~25% MgO: 5~10 % K 2 B: 0.1 to 0.2% is exemplified. This result is based on the experimental results shown in Table 1. Among the test items shown in Table 1, in the present invention, fire resistance, high temperature peelability and lubricity are particularly important.
また、後述するように、本発明にかかる潤滑剤にさら
に骨材を加えて使用する場合には、Al2O3、SiO2のどち
らか一方、または両方の含有量を10％程度とするととも
に、Na2SiO3を５〜10％程度とし、さらにMgO、K2Bは添
加しなくてもよい。Further, as will be described later, when the lubricant according to the present invention is further used with an aggregate, the content of either one of Al 2 O 3 and SiO 2 or both is set to about 10%. , Na 2 SiO 3 to about 5 to 10%, and MgO and K 2 B may not be added.
すなわち、本発明の潤滑剤の各成分の配合割合は、使
用成分の種類に応じて、所望の潤滑性能が得られるよう
に、当業者が実験により決定することができる。That is, the blending ratio of each component of the lubricant of the present invention can be experimentally determined by those skilled in the art so as to obtain a desired lubricating performance depending on the type of components used.
このようにして、たとえば熱間管圧延におけるガイド
シュー疵の発生を防止するのに好適な潤滑剤を製造する
ことができる。 In this way, it is possible to manufacture a lubricant suitable for preventing the occurrence of guide shoe defects in hot tube rolling, for example.
そして、このようにして得られる潤滑剤の使用は、圧
延前の被圧延材の表面に塗布しておくだけでよい。この
ようにして、熱間管圧延におけるガイドシュー疵の発生
を防止することができる。The lubricant thus obtained may be used only by applying it to the surface of the material to be rolled before rolling. In this way, it is possible to prevent the occurrence of guide shoe defects during hot tube rolling.
ところで、得られた本発明にかかる潤滑材中のFe3O4
の平均粒径は0.5μｍ以下であるため、そのまま用いる
と強度が不足し耐久性が足りないことがある。By the way, Fe 3 O 4 in the obtained lubricant according to the present invention
Since the average particle size is 0.5 μm or less, if used as it is, the strength may be insufficient and the durability may be insufficient.
一般的に潤滑材は、その平均粒径が細か過ぎて、１μ
ｍ未満となると塗布乾燥時（加熱時）に鋼材への密着性
が不足し容易に剥がれてしまう。すなわち、本発明によ
り得られるが如くの潤滑剤は、工具（ガイドシュー）と
被圧延材との間にメカニカルに巻き込まれることにより
効果を発揮する。したがって、粒径が細かすぎると巻き
込み性そのものの効率が悪くなる。Generally, the average particle size of a lubricant is too small,
If it is less than m, the adhesiveness to the steel material is insufficient at the time of coating and drying (during heating), and peeling off easily occurs. That is, the lubricant as obtained by the present invention exerts its effect by being mechanically caught between the tool (guide shoe) and the material to be rolled. Therefore, if the particle size is too small, the efficiency of the entrainment itself becomes poor.
一方、その粒径が粗過ぎて、200μｍ超となると、塗
布時に剥がれ易くビレット加熱しても脱落し易くなって
しまう。したがってガイドシュー疵対策に最終的に供さ
れる潤滑剤の量が少なくなってしまう。また、焼結した
塊が目に見える押さえ込み疵を誘発してしまう。したが
って、本発明により得られる潤滑剤の粒径は、１〜200
μｍであることが望ましい。特に好ましくは１〜100μ
ｍであり、100μｍを超えるとあばた疵が発生すること
がある。On the other hand, if the particle size is too coarse and exceeds 200 μm, the particles tend to peel off during coating and easily drop off even when the billet is heated. Therefore, the amount of the lubricant finally provided for the guide shoe flaw reduction becomes small. Also, the sintered mass induces visible pressing defects. Therefore, the particle size of the lubricant obtained by the present invention is from 1 to 200.
μm is desirable. Particularly preferably 1 to 100 μ
m, and if it exceeds 100 μm, pecking defects may occur.
なお、本発明者らの検討により得られた潤滑剤の粒度
と塗布時安定性、加熱時安定性、転送時密着性、ガイド
シュー疵発生程度および押さえ込み疵の発生程度との関
係の傾向を第２表にまとめて示す。It should be noted that the tendency of the relationship between the particle size of the lubricant and the stability during application, the stability during heating, the adhesiveness during transfer, the degree of guide shoe flaws, and the degree of pressing flaws, which were obtained by the study by the present inventors, are shown below. The results are summarized in Table 2.
なお、これらの判断基準は下記にまとめて示す。ま
た、これらの判断基準に基づいて、○（優）、△
（良）、×（不可）の三段階の評価を行った。 The criteria for these judgments are summarized below. In addition, based on these criteria, ○ (excellent), △
The evaluation was performed in three grades of (good) and x (impossible).
塗布時安定性：乾燥後（２時間後）ビレット表面より剥
離・脱落しない。Stability during coating: Does not peel off or fall off the billet surface after drying (after 2 hours).
加熱時安定性：加熱炉装入後、加熱時も含めて剥離・脱
落しない。Stability during heating: Does not peel off or fall off even after heating after charging in a heating furnace.
転送時安定性：加熱炉装入、抽出、転送コンベア、スキ
ッド上の衝撃を加えられたときにも脱落しない。Stability during transfer: Does not fall off when the furnace is charged, extracted, transferred on conveyor, or impacted on skids.
ガイドシュー疵：ガイドシュー上焼付疵を防止できる。
［ステンレス鋼（例;SUS304鋼）５本以上圧延時］ 押さえ込み疵：ビレットの圧延後パイプ表面に本発明の
潤滑剤が残存しない。Guide shoe flaw: Prevents seizure flaws on the guide shoe.
[When rolling 5 or more stainless steels (eg, SUS304 steel)] Depression flaw: The lubricant of the present invention does not remain on the pipe surface after billet rolling.
ここで第２表の従来例は、特開昭61−223096号公報に
記載されている潤滑剤である。Here, the conventional examples shown in Table 2 are the lubricants described in JP-A-61-223096.
また、酸洗廃液から製造された潤滑剤に骨材を重量比
で1:3〜1:5の割合で配合して潤滑剤として用いることも
本発明においては好ましい。骨材を加えることにより、
潤滑材の耐久性、耐火性を向上させるとともに、剥離性
をも向上させることができるからである。なお、骨材の
粒径は、細かすぎると粉砕のための工数が多くなり、ま
た骨材を加える効果がなく、粗すぎると疵が発生し塗布
性が悪化するため、50〜200μｍであることが望まし
い。Further, it is also preferable in the present invention that the lubricant produced from the pickling waste liquid is mixed with the aggregate at a weight ratio of 1: 3 to 1: 5 and used as the lubricant. By adding aggregate,
This is because it is possible to improve the durability and fire resistance of the lubricant as well as the peelability. If the particle size of the aggregate is too fine, the number of steps for crushing will be large, and there is no effect of adding the aggregate, and if it is too coarse, scratches will occur and the coatability will deteriorate, so it should be 50-200 μm. Is desirable.
さらに、本発明を実施例とともに詳述するが、これは
あくまでも本発明の例示であり、これにより本発明が限
定されるものではない。Furthermore, the present invention will be described in detail with reference to examples, but this is merely an example of the present invention, and the present invention is not limited thereby.
実施例 熱延工場の鉄鋼を酸洗した後の酸洗廃液をタンクに入
れ、Ca（OH）２を投入し、ノズルより高温蒸気と空気と
を吹き込み、Fe3O4とした後、静置沈澱させて、タンク
下部のバルブよりFe3O4を主成分とした沈澱液を脱水機
（遠心脱水機、真空濾過機）により脱水した後、タンク
に移し、インペラーにより撹拌しながら水道水を注入し
ながら撹拌・水洗した後、静置沈澱して、さらに脱水
し、水分60〜70％の含水Fe3O4スラリーとした後、Al
2O3、SiO2およびMgOを加え、混練配合し、粘着成分Na2S
iO3を加えた後、混練し、本発明にかかる潤滑剤とし
た。Example A pickling waste liquid after pickling steel in a hot rolling mill is put in a tank, Ca (OH) 2 is added, high-temperature steam and air are blown from a nozzle to make Fe 3 O 4 , and then allowed to stand. After precipitation, the precipitation liquid containing Fe 3 O 4 as the main component was dehydrated from the valve at the bottom of the tank using a dehydrator (centrifugal dehydrator, vacuum filter), then transferred to a tank, and tap water was added while stirring with an impeller. After stirring and washing with water, the solution was allowed to settle by standing and then dehydrated to form a water-containing Fe 3 O 4 slurry with a water content of 60 to 70%.
2 O 3 , SiO 2 and MgO were added, kneaded and mixed, and the adhesive component Na 2 S
After adding iO 3 , the mixture was kneaded to obtain a lubricant according to the present invention.
上記潤滑剤（平均粒径0.3μｍ）と鉱石を粉石した骨
材（平均粒径50μｍ）とを1:4の割合で配合し、最終的
に潤滑剤とした後、マンネスマン式製管法により熱間管
圧延する前にビレット表面に潤滑剤を厚さ1mm程度塗布
し、熱間圧延したところ、ガイドシュー疵も発生せず、
外観の良好なパイプを得ることができた。The above lubricant (average particle size 0.3 μm) and aggregate of ore powder (average particle size 50 μm) were mixed in a ratio of 1: 4, and finally used as a lubricant, and then by the Mannesmann pipe manufacturing method. Prior to hot tube rolling, a lubricant was applied to the billet surface to a thickness of about 1 mm and hot rolling was performed, and guide shoe flaws did not occur.
A pipe with a good appearance could be obtained.
（発明の効果） 以上詳述したように、本発明により、たとえば熱間管
圧延におけるガイドシュー疵の発生を防止するのに好適
な潤滑剤を得ることができる。(Effects of the Invention) As described in detail above, according to the present invention, it is possible to obtain a lubricant suitable for preventing the occurrence of guide shoe defects in hot tube rolling, for example.
かかる効果を有する本発明の実用上の意義は極めて著
しい。The practical significance of the present invention having such effects is extremely remarkable.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｃ１０Ｍ 125:26 103:06 ） Ｃ１０Ｎ 10:02 10:04 10:06 10:16 20:06 40:24 50:02 50:08 70:00 ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 6 Identification code Office reference number FI technical display location C10M 125: 26 103: 06) C10N 10:02 10:04 10:06 10:16 20:06 40 : 24 50:02 50:08 70:00
Claims (2)
酸化鉄（Fe3O4）と耐火成分と粘結剤と水とを混練して
なる潤滑剤。1. A lubricant obtained by kneading magnetic iron oxide (Fe 3 O 4 ) obtained from a pickling waste liquid after pickling iron and steel, a refractory component, a binder and water.
の重量割合で混練してなる潤滑剤。2. The lubricant according to claim 1 and the aggregate are 1: 3-5.
Lubricant made by kneading in the weight ratio of.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1228975A JP2556142B2 (en) | 1989-09-04 | 1989-09-04 | lubricant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1228975A JP2556142B2 (en) | 1989-09-04 | 1989-09-04 | lubricant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0391596A JPH0391596A (en) | 1991-04-17 |
| JP2556142B2 true JP2556142B2 (en) | 1996-11-20 |
Family
ID=16884806
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1228975A Expired - Lifetime JP2556142B2 (en) | 1989-09-04 | 1989-09-04 | lubricant |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2556142B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07112564B2 (en) * | 1987-09-28 | 1995-12-06 | 日新製鋼株式会社 | Lubricant for hot rolling of stainless steel |
| JP2638317B2 (en) * | 1991-01-10 | 1997-08-06 | 住友金属工業株式会社 | Lubricant for hot tube rolling and method for preventing seizure of hot rolled tube |
| EP1997872B1 (en) * | 2006-03-14 | 2014-06-11 | Nippon Steel & Sumitomo Metal Corporation | Lubricant for hot plastic working |
| CN107460022B (en) * | 2017-08-08 | 2020-01-10 | 大连海事大学 | Coprecipitation method for preparing chrysotile and Fe3O4Method for compounding lubricating oil additive |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS608276B2 (en) * | 1981-07-16 | 1985-03-01 | 日本黒鉛工業株式会社 | Water-based lubricant for hot rolling and hot rolling method using the same |
| JPS61223096A (en) * | 1985-03-28 | 1986-10-03 | Sumitomo Metal Ind Ltd | Lubricant for hot working of steel |
-
1989
- 1989-09-04 JP JP1228975A patent/JP2556142B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0391596A (en) | 1991-04-17 |
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