JPH0672746A - Method for reforming steel making slag - Google Patents
Method for reforming steel making slagInfo
- Publication number
- JPH0672746A JPH0672746A JP22614692A JP22614692A JPH0672746A JP H0672746 A JPH0672746 A JP H0672746A JP 22614692 A JP22614692 A JP 22614692A JP 22614692 A JP22614692 A JP 22614692A JP H0672746 A JPH0672746 A JP H0672746A
- Authority
- JP
- Japan
- Prior art keywords
- slag
- acid
- treatment
- reforming
- free cao
- 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.)
- Withdrawn
Links
- 239000002893 slag Substances 0.000 title claims abstract description 51
- 238000009628 steelmaking Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims description 18
- 238000002407 reforming Methods 0.000 title claims description 13
- 239000002253 acid Substances 0.000 claims abstract description 28
- 239000002699 waste material Substances 0.000 claims abstract description 16
- 239000010802 sludge Substances 0.000 claims abstract description 12
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 10
- 239000010959 steel Substances 0.000 claims abstract description 10
- 238000010306 acid treatment Methods 0.000 claims abstract description 6
- 150000007513 acids Chemical class 0.000 abstract description 3
- 230000036571 hydration Effects 0.000 abstract description 3
- 238000006703 hydration reaction Methods 0.000 abstract description 3
- 238000007598 dipping method Methods 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract 4
- 229910052742 iron Inorganic materials 0.000 abstract 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 2
- LFYJSSARVMHQJB-QIXNEVBVSA-N bakuchiol Chemical compound CC(C)=CCC[C@@](C)(C=C)\C=C\C1=CC=C(O)C=C1 LFYJSSARVMHQJB-QIXNEVBVSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000005097 cold rolling Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 239000004021 humic acid Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B5/00—Treatment of metallurgical slag ; Artificial stone from molten metallurgical slag
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、転炉スラグ等の遊離Ｃ
ａＯを含む製鋼スラグの有効利用促進のための、非常に
低コストで効率的な改質方法に関するものである。BACKGROUND OF THE INVENTION The present invention relates to free C in converter slag and the like.
The present invention relates to a very low cost and efficient reforming method for promoting effective utilization of steelmaking slag containing aO.
【０００２】[0002]
【従来の技術】転炉スラグ等の製鋼スラグは、遊離Ｃａ
Ｏを多く含むために水と接触してＣａＯがＣａ（ＯＨ）
2 となり、そのとき、ＣａＯの体積は約２倍に膨張す
る。このようなスラグを路盤材に利用した場合、膨張に
よりスラグが徐々に崩壊し、そのために路面に凹凸が生
じ車輌の走行に支障をきたすことになる。2. Description of the Related Art Steelmaking slag such as converter slag is free of Ca.
Since it contains a large amount of O, CaO becomes Ca (OH) upon contact with water.
2 , at which time the volume of CaO expands about twice. When such a slag is used as a roadbed material, the slag gradually collapses due to expansion, which causes unevenness on the road surface and hinders the running of the vehicle.
【０００３】この製鋼スラグの異常膨張の原因である遊
離ＣａＯを減少させるために以下の二つの方策が採られ
ている。 （１）エージング処理 徐冷した製鋼スラグを粗砕して粒度調整後、屋外にて山
積みして３〜６カ月以上放置し、雨水、大気中の水分、
ＣＯ2 等により水和・炭酸化反応等を行わせて遊離Ｃａ
Ｏを安定化させる大気エージング処理方法である。この
方法の問題点はエージングに非常に長時間を要すること
であり、そのために製鉄所内に非常に広いスペースが必
要であるという点にある。 （２）熱間改質処理 溶融状態の製鋼スラグに珪酸質材料等を添加して、遊離
ＣａＯをＳｉＯ2 ，Ａｌ2 Ｏ3 等と反応させて膨張しな
い安定鉱物相に変える方法である。この方法の問題点
は、改質処理コストが高くつくことである。The following two measures have been taken in order to reduce the free CaO which is the cause of the abnormal expansion of this steelmaking slag. (1) Aging treatment The slowly cooled steelmaking slag is roughly crushed and the particle size is adjusted, and then piled outdoors and left for 3 to 6 months or longer. Rainwater, atmospheric moisture,
Free Ca by hydration / carbonation reaction with CO 2 etc.
It is an atmospheric aging treatment method for stabilizing O 2. The problem with this method is that aging takes a very long time, which requires a very large space in the steel mill. (2) Hot reforming treatment This is a method of adding silicic material or the like to molten steelmaking slag and reacting free CaO with SiO 2 , Al 2 O 3 or the like to convert it into a stable mineral phase that does not expand. The problem with this method is that it is expensive to modify.
【０００４】以上の問題点を改善するために、特公昭５
２−４４２８１号公報、特開昭５８−１６７７０９号公
報に開示される技術は、フミン酸、硫酸等により遊離Ｃ
ａＯを安定な塩類に変えてエージング処理の省略を意図
したものである。しかし、遊離ＣａＯの製鋼スラグ内で
の存在状態は一様ではなく、スラグの粗粒内に取り込ま
れたりしており、これらの方法では、低コストで、か
つ、効率的に遊離ＣａＯを安定化させることはできなか
った。In order to improve the above problems, Japanese Patent Publication No.
The techniques disclosed in JP-A-2-44281 and JP-A-58-167709 are free C by humic acid, sulfuric acid and the like.
It is intended to replace aO with a stable salt and omit the aging treatment. However, the state of existence of free CaO in the steelmaking slag is not uniform, and it is incorporated in the coarse particles of the slag. With these methods, it is possible to stabilize free CaO efficiently at low cost. I couldn't let you do it.
【０００５】また、特開昭５８−１６７７０９号公報に
開示される方法の場合、濃硫酸（３６規定（Ｎ））を使
用しているために酸として強すぎて、遊離ＣａＯのみな
らず他のＣａＯを含む結晶相、例えばダイカルシウムシ
リケート（２ＣａＯ・ＳｉＯ 2 ）、トリカルシウムシリ
ケート（３ＣａＯ・ＳｉＯ2 ）等も溶解して、改質効率
が悪く、かつ、改質のためのコストも高くつくことが問
題であった。Further, in Japanese Patent Laid-Open No. 58-167709,
In the case of the disclosed method, concentrated sulfuric acid (36 N (N)) is used.
Since it is used as an acid, it is too strong,
But other crystalline phases containing CaO, such as dicalcium
Replicate (2CaO ・ SiO 2 ), Tricalcium sili
Kate (3CaO ・ SiO2 ) Etc. are also dissolved and reforming efficiency
Is bad and the cost for reforming is high.
It was the title.
【０００６】[0006]
【発明が解決しようとする課題】本発明は上記従来技術
の問題点を解決し、低コスト、かつ、効率的な製鋼スラ
グ改質方法を提供するものである。SUMMARY OF THE INVENTION The present invention solves the above-mentioned problems of the prior art and provides a low cost and efficient steelmaking slag reforming method.
【０００７】[0007]
【課題を解決するための手段】本発明における製鋼スラ
グ改質方法は、転炉等で発生した遊離ＣａＯを含む製鋼
スラグを、鉄鋼工場の酸処理工程において発生する廃酸
及び／又は酸スラッジを用いて処理することにより、遊
離ＣａＯを安定な中和塩に変える等してスラグから除去
したり、あるいは、スラグ中に残存させたりして改質す
ることを特徴としている。そのための改質処理条件とし
て、廃酸、酸スラッジを用いてｐＨを−１〜４、温度を
６０℃以上とする。The method for reforming steelmaking slag according to the present invention uses a steelmaking slag containing free CaO generated in a converter or the like to remove waste acid and / or acid sludge generated in an acid treatment process of a steel factory. It is characterized in that free CaO is removed from the slag by changing it into a stable neutralized salt by the treatment with the use, or is left in the slag for modification. As a modification treatment condition therefor, waste acid and acid sludge are used to adjust the pH to -1 to 4 and the temperature to 60 ° C or higher.
【０００８】[0008]
【作用】本発明者らは、前記改質処理技術に関して種々
検討した結果、鉄鋼工場の酸処理工程から発生する廃
酸、酸スラッジを有効利用することにより、非常に低コ
ストで、かつ、迅速に改質する方法を見出し、本発明を
完成した。本発明において、遊離ＣａＯを含む製鋼スラ
グは転炉スラグに限定されることはなく、遊離ＣａＯを
含む、例えば予備処理スラグから製鋼段階での取鍋スラ
グ、連鋳造塊スラグ、さらに電気炉スラグまで含まれ
る。As a result of various investigations on the above-mentioned modification treatment technology, the present inventors have made effective use of waste acid and acid sludge generated from the acid treatment process of a steel factory, resulting in very low cost and rapid The present invention has been completed by finding a method for modifying the above. In the present invention, the steelmaking slag containing free CaO is not limited to the converter slag, and includes free CaO, for example, from pretreatment slag to ladle slag at the steelmaking stage, continuous cast slag, and electric furnace slag. included.
【０００９】本発明においては、このような遊離ＣａＯ
を含む製鋼スラグを、鉄鋼工場の酸処理工程で発生する
廃酸及び／又は酸スラッジで処理することにより、遊離
ＣａＯの水和による異常膨張を抑え得たものである。本
発明に用いられる廃酸、酸スラッジの種類としては、鉄
鋼工場の酸処理工程から発生する限り特に限定されない
が、本発明において特に好適に用いられるものとして、
鉄鋼工場の熱間圧延、冷間圧延工程のピックリングで発
生する硫酸、塩酸等の無機酸による廃酸、酸スラッジが
好適である。本発明においては、このような廃酸、酸ス
ラッジを用いｐＨを−１〜４の範囲内に限定するが、こ
の範囲内に限定するのは、ｐＨが−１（水素イオン濃度
として１０規定（Ｎ））よりも小さいと、酸性が強すぎ
て製鋼スラグ中の遊離ＣａＯのみならず、他の安定なＣ
ａＯの結晶相、例えば２ＣａＯ・ＳｉＯ2 相等を溶解し
てしまい、遊離ＣａＯの安定化のためには効率がよくな
いからであり、また、逆にｐＨ４（水素イオン濃度とし
て１０-4規定（Ｎ））よりも酸性が弱くなると、遊離Ｃ
ａＯを迅速に安定化させることができなくなるからであ
る。In the present invention, such free CaO
The abnormal expansion due to the hydration of free CaO can be suppressed by treating the steelmaking slag containing slag with the waste acid and / or acid sludge generated in the acid treatment step of the steel factory. The type of waste acid and acid sludge used in the present invention is not particularly limited as long as it is generated from the acid treatment step of a steel plant, but as those particularly preferably used in the present invention,
Preference is given to waste acids and acid sludges due to inorganic acids such as sulfuric acid and hydrochloric acid, which are generated in the pickling of hot rolling and cold rolling processes in steel plants. In the present invention, such waste acid and acid sludge are used to limit the pH within the range of -1 to 4, but the range is limited to the pH of -1 (the hydrogen ion concentration is 10 N ( If it is smaller than N)), the acidity is too strong and not only free CaO in the steelmaking slag but also other stable C
crystal phase of aO-, for example would be dissolved 2CaO · SiO 2 phase etc., in order to stabilize the free CaO is because efficiency is not good, also contrary to pH 4 (10 -4 defined as the hydrogen ion concentration (N )) Less acidic than free C
This is because aO cannot be stabilized quickly.
【００１０】本発明においては、前述の廃酸及び／又は
酸スラッジを用い６０℃以上の温度で遊離ＣａＯを含む
製鋼スラグを処理するが、温度を６０℃以上に限定する
のは、反応速度を上げて遊離ＣａＯを効率的に無機酸の
中和塩にするためである。転炉スラグ等の製鋼スラグ中
の遊離ＣａＯの存在状態としては、スラグ塊の表面に存
在したり、塊の内部に存在したりして、その存在状態は
多様である。そのために路盤材として利用した場合の膨
張現象を非常に複雑なものにしている。本発明の場合に
は廃酸及び／又は酸スラッジを用い、ｐＨ−１〜４、温
度６０℃以上で処理することにより、スラグ塊の内部に
存在する遊離ＣａＯも効率的に安定化することができ
る。In the present invention, the steelmaking slag containing free CaO is treated at a temperature of 60 ° C. or higher using the above-mentioned waste acid and / or acid sludge, but the temperature is limited to 60 ° C. or higher because the reaction rate is limited. This is to raise the free CaO efficiently into a neutralized salt of an inorganic acid. As the existing state of free CaO in steelmaking slag such as converter slag, it exists on the surface of the slag lump or inside the lump, and its existing state is diverse. Therefore, the expansion phenomenon is extremely complicated when used as a roadbed material. In the case of the present invention, by using waste acid and / or acid sludge at pH -1 to 4 and at a temperature of 60 ° C or higher, free CaO existing inside the slag mass can also be efficiently stabilized. it can.
【００１１】なお、本発明における処理は、浸漬処理が
好適に用いられる。当然ながら、本発明の効率をより高
くするためには、処理スラグの粒径を小さくした方がよ
く、好適なスラグ粒径は１０ｍｍ以下である。また、本
発明の場合、前述の廃酸、酸スラッジに加えて、さら
に、新鮮な硫酸、塩酸等を配合してｐＨを−１〜４に調
整して製鋼スラグの改質処理に適用することもできる。As the treatment in the present invention, dipping treatment is preferably used. As a matter of course, in order to further increase the efficiency of the present invention, it is better to reduce the particle size of the treated slag, and the preferable slag particle size is 10 mm or less. In addition, in the case of the present invention, in addition to the above-mentioned waste acid and acid sludge, fresh sulfuric acid, hydrochloric acid, etc. are further mixed to adjust the pH to -1 to 4 and applied to the reforming treatment of the steelmaking slag. You can also
【００１２】[0012]
【実施例】１０ｍｍ以下に破砕した磁選後の転炉スラグ
を大量に採取し、化学分析を行った。表１にその結果を
示す。遊離ＣａＯの分析値は６．５ｗｔ％、塩基度（Ｃ
ａＯ／ＳｉＯ2 ）は４．１の転炉スラグであった。この
スラグを表２に示す製鋼工場で発生する廃酸、酸スラッ
ジを用いて、同表中に示す種々の温度、ｐＨ条件にて前
述のスラグを浸漬処理した。処理するスラグ量は１０ｋ
ｇずつとし、浸漬処理時間をそれぞれ５時間とした。処
理後、遊離ＣａＯの分析、水浸膨張試験後の膨張率の測
定を行い、転炉スラグの改質後の評価を行った。Example A large amount of converter slag after magnetic separation crushed to a size of 10 mm or less was collected and subjected to chemical analysis. The results are shown in Table 1. The analytical value of free CaO is 6.5 wt% and the basicity (C
aO / SiO 2 ) was 4.1 converter slag. This slag was subjected to immersion treatment using the waste acid and acid sludge generated in the steelmaking plant shown in Table 2 at various temperatures and pH conditions shown in the same table. The amount of slag to be processed is 10k
g, and the immersion treatment time was 5 hours. After the treatment, free CaO was analyzed and the expansion coefficient after the water immersion expansion test was measured to evaluate the converter slag after reforming.
【００１３】表２から明らかなように、本発明によれば
従来技術の比較例と比べて低処理コストで、改質処理後
の遊離ＣａＯの分析値は低いレベルになっている。遊離
ＣａＯは、ほとんど、廃硫酸の場合にＣａＳＯ4 、廃塩
酸の場合にＣａＣｌ2 となって安定化し、表２に示すよ
うに本発明の実施例の場合、改質処理後スラグの水浸膨
張試験による膨張率も路盤材用鉄鋼スラグの品質規格で
ある１．５％以下を満足している。As is clear from Table 2, according to the present invention, the analysis value of free CaO after the reforming treatment is at a low level at a low treatment cost as compared with the comparative example of the prior art. Most of the free CaO is stabilized with CaSO 4 in the case of waste sulfuric acid and CaCl 2 in the case of waste hydrochloric acid, and as shown in Table 2, in the case of the examples of the present invention, the water immersion expansion of the slag after the reforming treatment is performed. The expansion coefficient by the test also satisfies the quality standard of 1.5% or less of the steel slag for roadbed materials.
【００１４】[0014]
【発明の効果】本発明の処理方法を採用すれば、転炉ス
ラグ等の遊離ＣａＯを含む製鋼スラグを、従来の改質処
理に比べて極めて低コストで、かつ、効率的に安定化で
き、路盤材等に適したスラグに改質することができる。EFFECTS OF THE INVENTION By adopting the treatment method of the present invention, steelmaking slag containing free CaO such as converter slag can be efficiently stabilized at an extremely low cost as compared with the conventional reforming treatment, It can be modified into slag suitable for roadbed materials.
【００１５】[0015]
【表１】 [Table 1]
【００１６】[0016]
【表２】 [Table 2]
───────────────────────────────────────────────────── フロントページの続き (72)発明者 野崎 努 千葉市中央区川崎町１番地 川崎製鉄株式 会社技術研究本部内 (72)発明者 天辰 正義 千葉市中央区川崎町１番地 川崎製鉄株式 会社第３別館内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Tsutomu Nozaki 1 Kawasaki-cho, Chuo-ku, Chiba City Technical Research Division, Kawasaki Steel Co., Ltd. (72) Masayoshi Tenshin, 1 Kawasaki-cho, Chuo-ku, Chiba 3 annex
Claims (1)
場の酸処理工程で発生する廃酸及び／又は酸スラッジを
用いて、ｐＨ−１〜４、温度６０℃以上で処理すること
を特徴とする製鋼スラグ改質方法。1. A steelmaking slag containing free CaO is treated at a pH of 1 to 4 and at a temperature of 60 ° C. or higher using waste acid and / or acid sludge generated in an acid treatment process of a steel factory. Steelmaking slag reforming method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22614692A JPH0672746A (en) | 1992-08-25 | 1992-08-25 | Method for reforming steel making slag |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22614692A JPH0672746A (en) | 1992-08-25 | 1992-08-25 | Method for reforming steel making slag |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0672746A true JPH0672746A (en) | 1994-03-15 |
Family
ID=16840583
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP22614692A Withdrawn JPH0672746A (en) | 1992-08-25 | 1992-08-25 | Method for reforming steel making slag |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0672746A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1992001567A1 (en) * | 1990-07-17 | 1992-02-06 | Presstek, Inc. | Control system for spark-discharge recording head |
| JP2001199749A (en) * | 2000-01-12 | 2001-07-24 | Kawasaki Steel Corp | Surface modification method for blast furnace slag and modified blast furnace slag |
| JP2008168289A (en) * | 2006-12-11 | 2008-07-24 | Sumitomo Metal Ind Ltd | Detoxification method of heavy metal-containing basic waste |
-
1992
- 1992-08-25 JP JP22614692A patent/JPH0672746A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1992001567A1 (en) * | 1990-07-17 | 1992-02-06 | Presstek, Inc. | Control system for spark-discharge recording head |
| JP2001199749A (en) * | 2000-01-12 | 2001-07-24 | Kawasaki Steel Corp | Surface modification method for blast furnace slag and modified blast furnace slag |
| JP2008168289A (en) * | 2006-12-11 | 2008-07-24 | Sumitomo Metal Ind Ltd | Detoxification method of heavy metal-containing basic waste |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A300 | Withdrawal of application because of no request for examination |
Free format text: JAPANESE INTERMEDIATE CODE: A300 Effective date: 19991102 |