JP2002180108A - Brittle compact and manufacturing method - Google Patents

Brittle compact and manufacturing method

Info

Publication number
JP2002180108A
JP2002180108A JP2001302116A JP2001302116A JP2002180108A JP 2002180108 A JP2002180108 A JP 2002180108A JP 2001302116 A JP2001302116 A JP 2001302116A JP 2001302116 A JP2001302116 A JP 2001302116A JP 2002180108 A JP2002180108 A JP 2002180108A
Authority
JP
Japan
Prior art keywords
brittle molded
brittle
weight
molded product
oil
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.)
Granted
Application number
JP2001302116A
Other languages
Japanese (ja)
Other versions
JP3774652B2 (en
Inventor
Masataka Ishihara
正孝 石原
Akio Maemoto
昭雄 前本
Mitsuma Matsuda
光馬 松田
Yoshihiro Kiyoo
良弘 清尾
Shoichi Kashino
彰一 樫野
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Koyo Seiko Co Ltd
Original Assignee
Koyo Seiko Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Koyo Seiko Co Ltd filed Critical Koyo Seiko Co Ltd
Priority to JP2001302116A priority Critical patent/JP3774652B2/en
Publication of JP2002180108A publication Critical patent/JP2002180108A/en
Application granted granted Critical
Publication of JP3774652B2 publication Critical patent/JP3774652B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B30PRESSES
    • B30BPRESSES IN GENERAL
    • B30B9/00Presses specially adapted for particular purposes
    • B30B9/32Presses specially adapted for particular purposes for consolidating scrap metal or for compacting used cars
    • B30B9/327Presses specially adapted for particular purposes for consolidating scrap metal or for compacting used cars for briquetting scrap metal

Abstract

PROBLEM TO BE SOLVED: To provide a brittle compact with which grinding swarf can be effectively recycled and also to provide its manufacturing method. SOLUTION: A flocculent agglomerate B which contains grinding swarf of ferrous metal and grinding fluid containing oil and water is compacted to prepare a brittle compact A where the grinding swarf in a fibrous state is sheared and excess water and oil are removed. It is effective to carry out the compaction of the brittle compact while using an auxiliary agent for solidification, such as colloidal silica, sodium silicate, aluminum phosphate and asphalt emulsion, or to impregnate the compact with the auxiliary agent for solidification.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】この発明は、脆性成形体及び
その製造方法に関し、特に、鉄系金属の研削切粉を有効
利用する技術に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a brittle compact and a method for producing the same, and more particularly, to a technique for effectively using ground metal chips of a ferrous metal.

【0002】[0002]

【従来の技術】軸受鋼や浸炭鋼等の鉄系金属を研削(以
下研磨、超仕上げ研磨及びラッピング等も含む概念とし
て使用する)した際に生じる切粉は、水分及び油分を含
有する研削液や砥粒等を含む綿状(繊維状)凝集体とし
て回収されている。この綿状凝集体は多量の純鉄を含む
ことから、例えば製鋼原料として再利用することが試み
られている。しかし、この綿状凝集体は多量の水分を含
有していることから、これを溶鉱炉にそのまま投入する
と、当該水分によって突沸(水蒸気爆発)が生じるとい
う問題を引き起こす。そこで、綿状凝集体中の水分を遠
心分離等によって除去することが考えられるが、この場
合には、綿状凝集体に含まれる油分も水分とともに除去
されて、綿状凝集体の自然発熱により研削切粉の成分で
ある純鉄が酸化鉄に変質する。このため、これを製鋼原
料として再利用するには還元する必要があり、還元剤の
使用等によりコスト高になる。
2. Description of the Related Art Chips generated when grinding ferrous metals such as bearing steel and carburized steel (hereinafter used as a concept including polishing, superfinishing and lapping) are grinding fluids containing water and oil. And a flocculent (fibrous) aggregate containing abrasive grains and the like. Since this flocculent aggregate contains a large amount of pure iron, it has been attempted to reuse it as, for example, a steelmaking raw material. However, since this flocculent agglomerate contains a large amount of water, if it is put into a blast furnace as it is, the water causes a problem of bumping (steam explosion). Therefore, it is conceivable to remove the water in the flocculent aggregate by centrifugation or the like.In this case, the oil contained in the flocculent aggregate is also removed together with the moisture, and the flocculent aggregate naturally generates heat. Pure iron, which is a component of grinding chips, is transformed into iron oxide. For this reason, in order to reuse this as a steelmaking raw material, it is necessary to reduce it, and the use of a reducing agent increases costs.

【0003】また、前記油分の付着した研削切粉は相互
に密着し難いことから、綿状凝集体を圧縮成形しても所
望の強度に固形化するのが困難である。さらに、炭素の
含有量が0.2重量%以上の鉄系金属の研削切粉を多量
に含む綿状凝集体については、圧縮時のスプリングバッ
クが大きいので、これを圧縮成形しても所望の強度に固
形化するのが困難である。したがって、圧縮成形した綿
状凝集体を溶鉱炉に投入しても、飛散しながら舞い上が
って、集塵機によって大半が回収されてしまうという問
題を生じる。さらに、前記綿状凝集体に含まれる繊維状
の研削切粉は、ハンマーミル等で粉砕することが困難で
あるので、綿状凝集体を細かくせん断して粉体にするこ
とができない。このため、綿状凝集体を卵形等のブリケ
ット等に加工することも困難である。したがって、前記
綿状凝集体は再利用することなく廃棄物処理業者に委託
して埋め立て処分されているのが実状である。
[0003] In addition, since the above-mentioned ground chips to which the oil component adheres hardly adhere to each other, it is difficult to solidify to a desired strength even if the flocculent aggregate is compression-molded. Further, the flocculent agglomerate containing a large amount of ground cuttings of an iron-based metal having a carbon content of 0.2% by weight or more has a large springback at the time of compression. It is difficult to solidify strongly. Therefore, even if the compression-molded flocculent aggregate is put into a blast furnace, it flies up while scattering and is mostly collected by the dust collector. Furthermore, since the fibrous ground chips contained in the flocculent aggregate are difficult to pulverize with a hammer mill or the like, the flocculent aggregate cannot be finely sheared into powder. For this reason, it is also difficult to process the flocculent aggregate into an egg-shaped briquette or the like. Therefore, the actual state is that the flocculent aggregate is disposed of by a waste disposal contractor without being reused.

【0004】[0004]

【発明が解決しようとする課題】しかし、このような綿
状凝集体の埋め立て処分は、資源の有効利用という観点
から好ましくない。また、環境悪化を引き起こすととも
に、廃棄コストが高くつくという問題もある。この発明
は、前記問題点に鑑みてなされたものであり、研削切粉
を有効に再利用することができる脆性成形体及びその製
造方法を提供することを目的とする。
However, such landfill disposal of flocculent aggregates is not preferable from the viewpoint of effective utilization of resources. In addition, there is a problem that the environment is deteriorated and the disposal cost is high. The present invention has been made in view of the above problems, and an object of the present invention is to provide a brittle molded body that can effectively reuse ground chips and a method of manufacturing the same.

【0005】[0005]

【課題を解決するための手段】前記目的を達成するため
のこの発明の脆性成形体は、鉄系金属の研削切粉と油分
及び水分を含有する研削液とを含む綿状凝集体を所定形
状に圧縮成形してなることを特徴としている(請求項
1)。このように構成された脆性成形体によれば、綿状
凝集体を圧縮成形したものであるので、繊維状の研削切
粉がせん断された脆性を有するものになる。また、残留
する油分によって研削切粉の成分である純鉄が酸化する
のが防止される。
The brittle compact of the present invention for achieving the above object is characterized by forming a flocculent agglomerate containing a grinding chip of an iron-based metal and a grinding fluid containing oil and moisture into a predetermined shape. (Claim 1). According to the brittle molded body configured as described above, since the flocculent agglomerate is formed by compression molding, the fibrous ground cutting chips are brittle by shearing. Further, the oxidation of pure iron, which is a component of the grinding chips, by the remaining oil is prevented.

【0006】前記脆性成形体は固形化補助剤で固形化し
たものであってもよく(請求項2)、この場合には、脆
性成形体を所望の強度に固形化することができる。前記
固形化補助剤は、コロイダルシリカ、珪酸ソーダ、燐酸
アルミニウム、アスファルト乳剤から選択される少なく
とも1種であるのが好ましく(請求項3)、これによ
り、油分を含有しているにもかかわらず強固に固形化さ
れた脆性成形体となる。前記脆性成形体の含油率は1〜
5重量%であるのが好ましく(請求項4)、この場合に
は、適度の硬さに固形化されているとともに、最小限の
残留油分によって研削切粉の成分である純鉄が酸化する
のを効果的に防止することができる。
The brittle molded article may be solidified with a solidification aid (claim 2). In this case, the brittle molded article can be solidified to a desired strength. The solidification aid is preferably at least one selected from colloidal silica, sodium silicate, aluminum phosphate, and asphalt emulsion (claim 3). It becomes a brittle molded body that has been solidified. The oil content of the brittle molded product is 1 to
Preferably, the content is 5% by weight (claim 4). In this case, while being solidified to an appropriate hardness, pure iron which is a component of the grinding chips is oxidized by a minimum residual oil content. Can be effectively prevented.

【0007】またこの発明の脆性成形体の製造方法は、
鉄系金属の研削切粉と油分及び水分を含有する研削液と
を含む綿状凝集体を圧縮成形して、繊維状の研削切粉が
せん断され且つ余剰の水分及び油分が除去された所定形
状の脆性成形体を得ることを特徴としている(請求項
5)。このように構成された脆性成形体の製造方法によ
れば、前記綿状凝集体の圧縮成形によって、従来せん断
が困難であった繊維状の研削切粉を容易にせん断するこ
とができる。また、前記圧縮成形を研削液に含まれてい
る油分を保持した状態で行うので、研削切粉の成分であ
る純鉄が酸化するのを防止することができる。
[0007] Further, the method for producing a brittle molded article of the present invention comprises:
Compression molding of flocculent agglomerates containing iron-based metal grinding chips and a grinding fluid containing oil and moisture, a predetermined shape in which fibrous grinding chips are sheared and excess moisture and oil are removed (Claim 5). According to the manufacturing method of the brittle molded body configured as described above, the compression molding of the flocculent agglomerates can easily shear the fibrous ground chips which have conventionally been difficult to shear. Further, since the compression molding is performed while retaining the oil content contained in the grinding fluid, it is possible to prevent the pure iron, which is a component of the grinding chips, from being oxidized.

【0008】前記脆性成形体の製造方法は、前記脆性成
形体に固形化補助剤を含浸させる工程をさらに含んでい
てもよく(請求項6)、この場合には、所望の強度に固
形化された脆性成形体を得ることができる。前記固形化
補助剤としては、コロイダルシリカ、珪酸ソーダ、燐酸
アルミニウムアスファルト乳剤から選択される少なくと
も1種を用いるのが好ましく(請求項7)、これによ
り、油分を含むにもかかわらずより強固に固形化された
脆性成形体を得ることができる。また、前記固形化補助
剤は2〜30重量%含浸させるのが好ましく(請求項
8)、これにより、より一層強固に固形化された脆性成
形体を得ることができる。
The method for producing a brittle molded product may further include a step of impregnating the brittle molded product with a solidification aid (claim 6). In this case, the brittle molded product is solidified to a desired strength. A brittle molded article can be obtained. As the solidification aid, it is preferable to use at least one selected from colloidal silica, sodium silicate, and aluminum phosphate asphalt emulsion (claim 7), whereby the solidification is enhanced even though oil is contained. A brittle molded article can be obtained. Further, it is preferable that the solidification aid is impregnated with 2 to 30% by weight (claim 8), whereby a brittle molded product which is more solidified can be obtained.

【0009】前記脆性成形体の製造方法においては、前
記綿状凝集体として含水率が50重量%を超えない範囲
に、含油率が10重量%を超えない範囲にそれぞれ調整
したものを用いるのが好ましい(請求項9)。これによ
り、前記綿状凝集体の運搬等の取り扱いが容易となると
ともに、圧縮成形のみによって脆性成形体の余剰の水分
及び油分を容易かつ適正に除去することができる。
In the method for producing a brittle molded article, it is preferable to use the flocculent aggregate which has been adjusted to a water content not exceeding 50% by weight and an oil content not exceeding 10% by weight. Preferred (claim 9). This facilitates handling such as transportation of the floc and the like, and allows easy and appropriate removal of excess moisture and oil content of the brittle molded body only by compression molding.

【0010】前記脆性成形体の製造方法においては、前
記脆性成形体の含水率を2〜12重量%、含油率を1〜
5重量%に調整するのが好ましい(請求項10)。この
場合には、脆性成形体を適度の硬さに固形化することが
できるとともに、最小限の残留油分によって研削切粉の
成分である純鉄が酸化するのを効果的に防止することが
できる。また、前記研削切粉としては、炭素を0.2重
量%以上含むものを用いてもよく(請求項11)、この
ようなスプリングバックの大きい研削切粉についても、
そのスプリングバックの影響を排除して前記圧縮成形に
より効果的にせん断することができる。
In the method for producing a brittle molded product, the brittle molded product has a water content of 2 to 12% by weight and an oil content of 1 to 12% by weight.
It is preferably adjusted to 5% by weight (claim 10). In this case, the brittle molded body can be solidified to an appropriate hardness, and the oxidation of pure iron, which is a component of the grinding chips, can be effectively prevented by the minimum residual oil content. . Further, as the grinding chips, those containing 0.2% by weight or more of carbon may be used (claim 11).
The effect of the springback can be eliminated to achieve effective shearing by the compression molding.

【0011】[0011]

【発明の実施の形態】以下、この発明の実施の形態につ
いて添付図面を参照しながら詳述する。図1はこの発明
の一実施形態に係る脆性成形体の製造方法を示す工程図
である。この脆性成形体Aの製造においては、まず鉄系
金属を研削加工する際に発生する研削切粉の綿状凝集体
B(図1(a)参照)を加圧圧縮して、当該綿状凝集体B
に含まれる研削液の成分である水分及び油分の含有量を
予備的に調整する。この綿状凝集体Bの加圧圧縮は、例
えばベルトコンベア1にて搬送しながら一対のロール2
間に挟み込むことにより行う(図1(b)参照)。但しこ
の水分及び油分の調整は、単なるエアー吹き付けやエア
ー圧縮により行う方法もある。この際、綿状凝集体B
は、含水率が50重量%を超えない範囲に、含油率が1
0重量%を超えない範囲にそれぞれ調整するのが好まし
く、これにより、綿状凝集体Bの搬送、貯蔵等の取り扱
いが容易となる。
Embodiments of the present invention will be described below in detail with reference to the accompanying drawings. FIG. 1 is a process chart showing a method for manufacturing a brittle molded body according to one embodiment of the present invention. In the production of the brittle compact A, first, the flocculent aggregate B (see FIG. 1 (a)) of the grinding chips generated when the ferrous metal is ground is compressed under pressure, and the flocculent coagulate B is formed. Gather B
Preliminarily adjust the contents of water and oil, which are components of the grinding fluid contained in the above. The pressurization and compression of the flocculent aggregate B is performed, for example, by a pair of rolls 2
It is performed by being sandwiched between them (see FIG. 1 (b)). However, there is a method of adjusting the water content and the oil content by simple air blowing or air compression. At this time, the flocculent aggregate B
Means that the oil content is not more than 50% by weight and the oil content is 1
It is preferable to adjust each of the amounts so as not to exceed 0% by weight, so that handling such as transportation and storage of the flocculent aggregate B becomes easy.

【0012】次に、水分及び油分の含有量が調整された
前記綿状凝集体Bを、成形型3を用いて例えばプレスに
より圧縮成形して脆性成形体Aを得る(図1(c)参
照)。この圧縮成形によって、綿状凝集体Bに含まれる
スパイラル繊維状の研削切粉がせん断される。また、余
剰の水分及び油分が除去されて、前記脆性成形体Aの含
水率が2〜12重量%に、含油率が1〜5重量%に調整
される。これにより、最小限の残留油分によって研削切
粉の成分である純鉄が酸化するのを効果的に防止するこ
とができる。また、前工程において綿状凝集体Bの含水
率が50重量%、含油率が10重量%をそれぞれ超えな
い範囲に予め調整されているので、前記脆性成形体Aの
水分及び油分の含有割合を圧縮成形のみによって容易か
つ適正に調整することができる。前記脆性成形体Aは、
円柱形、球形、角柱形等の取り扱いの容易な形状に形成
されているとともに、搬送時等に崩壊しない程度の強度
に固められている。
Next, the flocculent agglomerate B having the adjusted water and oil content is compression molded by, for example, pressing using a molding die 3 to obtain a brittle molded body A (see FIG. 1 (c)). ). By this compression molding, the spiral fiber-shaped ground chips contained in the flocculent aggregate B are sheared. Further, excess water and oil are removed, and the water content of the brittle molded product A is adjusted to 2 to 12% by weight, and the oil content is adjusted to 1 to 5% by weight. Thereby, it is possible to effectively prevent the oxidation of pure iron, which is a component of the grinding chips, with a minimum residual oil content. Also, since the water content of the flocculent agglomerate B is adjusted in advance to a range not exceeding 50% by weight and the oil content not exceeding 10% by weight, the water content and the oil content of the brittle molded product A are reduced. It can be easily and properly adjusted only by compression molding. The brittle molded body A is
It is formed in a shape that is easy to handle, such as a column, a sphere, and a prism, and is hardened to such a degree that it does not collapse during transportation or the like.

【0013】次いで、前記脆性成形体Aに、液状の固形
化補助剤Dを含浸させる。この固形化補助剤Dの含浸
は、例えば脆性成形体Aをベルトコンベア7にて搬送し
ながら、タンク8に注入した前記固形化補助剤Dに浸漬
させることにより行う(図1(d)参照)。この実施の形
態に用いる固形化補助剤Dとしては、コロイダルシリ
カ、珪酸ソーダ、燐酸アルミニウム、アスファルト乳剤
から選択される少なくとも1種を用いるのが好ましく、
これにより、脆性成形体Aを容易且つ強固に固形化する
ことができる。また、これら固形化補助剤は2〜30重
量%含浸させるのが好ましく、これにより、より一層強
固に固形化された脆性成形体Aを得ることができる。
Next, the brittle compact A is impregnated with a liquid solidification aid D. The impregnation with the solidification aid D is performed, for example, by immersing the brittle molded body A in the solidification aid D injected into the tank 8 while conveying the brittle molded body A on the belt conveyor 7 (see FIG. 1D). . As the solidification aid D used in this embodiment, it is preferable to use at least one selected from colloidal silica, sodium silicate, aluminum phosphate, and asphalt emulsion,
Thereby, the brittle molded body A can be easily and firmly solidified. Further, it is preferable to impregnate these solidification aids with 2 to 30% by weight, so that the brittle molding A solidified more firmly can be obtained.

【0014】以上により得られた脆性成形体Aは、研削
液の油分の一部を加工中を含めて常に保持しているの
で、研削切粉の成分である純鉄の酸化が効果的に防止さ
れている。このため、特に製鋼原料用のブリケットの材
料として好適に再利用することができる。例えば、図2
に示すように、前記固形化補助剤Dを含浸させた脆性成
形体Aを(図2(a)参照)養生(乾燥)してその含有水
分を除去することにより(図2(b)参照)、製鋼原料用
のブリケットGを得ることができる(図2(c)参照)。
この養生は2日間程度行うのが含有水分を確実に除去す
ることができるので好ましい。前記養生に際しては、常
温乾燥の他、エアーによる吹き付け乾燥を行ってもよ
い。
Since the brittle compact A obtained as described above always retains a part of the oil of the grinding fluid even during machining, the oxidation of pure iron, which is a component of grinding chips, is effectively prevented. Have been. Therefore, it can be suitably reused particularly as a briquette material for a steelmaking raw material. For example, FIG.
As shown in FIG. 2, the brittle compact A impregnated with the solidification aid D is cured (dried) (see FIG. 2 (a)) to remove the water content (see FIG. 2 (b)). Thus, a briquette G for a steelmaking raw material can be obtained (see FIG. 2 (c)).
It is preferable to carry out this curing for about two days because the water content can be surely removed. In the curing, spray drying with air may be performed in addition to drying at room temperature.

【0015】以上により得られたブリケットGは、脆性
成形体Aを乾燥させているものであるので、そのまま溶
鉱炉に投入しても突沸が生じたり舞い上がって排出され
たりするおそれがない。また、研削液の油分の一部を常
に保持した状態で加工しているので、純鉄の酸化が効果
的に防止されている。例えば軸受鋼(SUJ−2)の研
削切粉を含む綿状凝集体Bを用いて製造されたブリケッ
トGについては、70重量%以上の純鉄を含むことが確
認されている。したがって、溶解歩留まりが90%以上
と非常に高く、高品質の製鋼原料として製鋼メーカに有
償で提供することができる。しかも、固形にて運搬その
他の取り扱いが容易である。また、前記ブリケットGの
製造方法は、綿状凝集体Bを粉砕して微細化する工程を
要することなく当該綿状凝集体Bを固形化することがで
きるので、ブリケットGを能率よく製造することができ
る。
The briquette G obtained as described above is obtained by drying the brittle molded body A, so that there is no danger of bumping or soaring even if it is put into a blast furnace as it is. Further, since the machining is performed while a part of the oil of the grinding fluid is always held, the oxidation of the pure iron is effectively prevented. For example, it has been confirmed that a briquette G manufactured using flocculent aggregate B containing ground cuttings of bearing steel (SUJ-2) contains 70% by weight or more of pure iron. Therefore, the melting yield is as high as 90% or more, and it can be provided as a high quality steelmaking raw material to a steelmaker for a fee. Moreover, it is easy to carry and other handling in solid form. In addition, the method for producing the briquette G can solidify the flocculent aggregate B without requiring a step of pulverizing and refining the flocculent aggregate B, so that the briquette G can be efficiently produced. Can be.

【0016】前記脆性成形体Aは固形化補助剤Dを含浸
させていないものであってもよく、この場合には、例え
ば以下に示す方法により製鋼原料用のブリケットGを製
造することができる。すなわち、まず図1(c)に示す圧
縮成形により得られた脆性成形体Aを、固形化補助剤D
とともに回転刃4を備えるチョッパー付きミキサー(又
はヘンシェル型ミキサー)5に投入して粉砕する(図3
(a)参照)。これにより脆性成形体Aの研削切粉をさら
に細かくせん断(仕上げせん断)して、純鉄からなる鉄
系粉末、油分及び固形化補助剤Dを含む粉体Eを得るこ
とができる(図3(b)参照)。前記鉄系粉末の長径は3
〜1000μm程度のものである。この脆性成形体Aの
粉砕に際しては、当該脆性成形体A中の繊維状の研削切
粉が予めせん断されているので、これを支障なく仕上げ
せん断することができる。この脆性成形体A中の繊維状
の研削切粉がせん断がされていない場合には、これをチ
ョッパー付きミキサー(又はヘンシェル型ミキサー)5
によって粉砕するのに長時間を要し、経済的にメリット
が得られないとともに、微細な鉄系粉末を得ることも難
しい。なお、この場合に用いる固形化補助剤としては、
米糠、サトウキビ等の廃糖蜜、芋澱粉やコーンスターチ
等の澱粉類、生石灰、コロイダルシリカ、珪酸ソーダ、
燐酸アルミニウム、酢酸ビニル汚泥、アスファルト乳
剤、ベントナイトのうちから選択される1種又は2種以
上が好適に使用される。特に、前記米糠及び廃糖蜜につ
いては、粉体Eの固形化を効果的に促進し、その価格も
安いことから固形化補助剤Dとしてきわめて好適であ
る。また、アスファルト乳剤は混練後、アスファルトと
水に分離すると粘結性が生じ、強度が発現する。このア
スファルト乳剤としては、アニオン系アスファルトが好
適に使用される。
The brittle compact A may not be impregnated with the solidification aid D. In this case, a briquette G for a steelmaking raw material can be produced, for example, by the following method. That is, first, the brittle molded product A obtained by compression molding shown in FIG.
Together with a chopper-equipped mixer (or Henschel-type mixer) 5 having a rotary blade 4 for pulverization (FIG. 3).
(a)). In this way, the ground cuttings of the brittle compact A are further finely sheared (finish shearing) to obtain a powder E containing an iron-based powder made of pure iron, an oil component, and a solidification aid D (FIG. 3 ( b)). The major axis of the iron-based powder is 3
About 1000 μm. At the time of pulverizing the brittle molded body A, since the fibrous ground cuttings in the brittle molded body A have been sheared in advance, they can be finish-sheared without any trouble. If the fibrous ground chips in the brittle molded body A are not sheared, they are mixed with a mixer with a chopper (or Henschel mixer) 5
It takes a long time to pulverize, and it is not economically advantageous, and it is also difficult to obtain a fine iron-based powder. In addition, as a solidification auxiliary used in this case,
Waste molasses such as rice bran and sugarcane, starches such as potato starch and corn starch, quicklime, colloidal silica, sodium silicate,
One or more selected from aluminum phosphate, vinyl acetate sludge, asphalt emulsion, and bentonite are preferably used. Particularly, the rice bran and molasses are very suitable as the solidification aid D because the solidification of the powder E is effectively promoted and the price is low. In addition, when the asphalt emulsion is kneaded and then separated into asphalt and water, caking is generated and the strength is developed. As the asphalt emulsion, an anionic asphalt is preferably used.

【0017】次に、所定量の前記粉体Eを、例えばロー
ル型成形機やシリンダ型成形機6を用いて圧縮成形して
(図3(c)参照)、多量の純鉄を含有するほぼピロー形
状のブリケットFを得る。この粉体Eの圧縮成形に際し
ては、前記固形化補助剤Dと粉体E中の水分とによっ
て、油脂が付着した鉄系粉末どうしを強固に結合させて
固形化することができる。特に、粉体Eとして水分5〜
6重量%、米糠4重量%及び廃糖蜜2重量%含むもの、
並びに水分7〜15重量%、酢酸ビニル汚泥2〜10重
量%含むものを用いる場合には、より強固に固形化され
たブリケットFを得ることができる。
Next, a predetermined amount of the powder E is compression-molded by using, for example, a roll-type molding machine or a cylinder-type molding machine 6 (see FIG. 3 (c)). A pillow-shaped briquette F is obtained. During the compression molding of the powder E, the iron-based powder to which the fat or oil has adhered can be firmly bound and solidified by the solidification aid D and the water in the powder E. In particular, as powder E, water 5
Containing 6% by weight, rice bran 4% by weight and molasses 2% by weight,
In addition, when a material containing 7 to 15% by weight of water and 2 to 10% by weight of vinyl acetate sludge is used, briquette F solidified more firmly can be obtained.

【0018】そして、圧縮成形直後のブリケットFに常
温又は冷却されたエアーを吹き付けてこれを急速冷却す
る(図3(d)参照)。これにより、当該ブリケットFを
容易且つ安定的に固形化することができる。その後、ブ
リケットFを養生(乾燥)してその含有水分を除去する
ことにより(図3(e)参照)、製鋼原料用のブリケット
Gを得ることができる(図3(f)参照)。この養生は2
日間程度行うのが含有水分を確実に除去することができ
るので好ましい。
Then, the briquette F immediately after compression molding is blown with room temperature or cooled air to rapidly cool it (see FIG. 3 (d)). Thereby, the briquette F can be easily and stably solidified. Thereafter, the briquette F is cured (dried) to remove the water content (see FIG. 3 (e)), thereby obtaining a briquette G for a steelmaking raw material (see FIG. 3 (f)). This curing is 2
It is preferable to carry out the treatment for about a day because the contained water can be surely removed.

【0019】前記した脆性成形体Aの製造方法は、炭素
を0.2重量%以上含む研削切粉を再利用するのに特に
好適に適用される。このような研削切粉は、スプリング
バックが大きく、固形化が困難であるが、この発明の図
1(c)で示す圧縮成形を適用することにより、スプリン
グバックの影響を排除して当該研削切粉を効果的にせん
断することができる。なお、炭素を0.2重量%以上含
む研削切粉の代表例としては、軸受鋼の研削切粉を挙げ
ることができる。
The above-described method for producing a brittle compact A is particularly suitably applied to the reuse of ground chips containing 0.2% by weight or more of carbon. Such grinding chips have a large springback and are difficult to solidify. However, by applying the compression molding of the present invention shown in FIG. The powder can be effectively sheared. As a typical example of the ground chips containing 0.2% by weight or more of carbon, ground chips of bearing steel can be given.

【0020】なお、前記脆性成形体Aの形状としては、
前記円柱形等のほか、卵形、アーモンド形、ラグビーボ
ール形等のような、周縁部に丸みを有し、周縁部から中
央部に向かって肉厚が漸次厚くなるほぼピロー形状であ
ってもよい(図4参照)。このような形状に成形するこ
とにより、圧縮荷重に強くより崩壊し難いとともに、角
部等における部分的な破損が生じ難いものになる。ま
た、この発明の脆性成形体Aは、粉砕して粉体にするこ
とにより、前記製鋼原料用のブリケットG以外に、焼結
金属用の粉末原料や、磁性材料用途としての樹脂等の添
加材としても再利用することができる。
The shape of the brittle molded body A is as follows.
In addition to the cylindrical shape and the like, an oval shape, an almond shape, a rugby ball shape, and the like, having a rounded peripheral portion, and a substantially pillow shape in which the thickness gradually increases from the peripheral portion toward the central portion. Good (see FIG. 4). By being formed into such a shape, it is strong against a compressive load and hardly collapses, and partial breakage at corners or the like hardly occurs. Further, the brittle molded body A of the present invention is pulverized into powder, so that, in addition to the briquette G for the steelmaking raw material, a powdered raw material for a sintered metal and an additive material such as a resin for a magnetic material use. Can also be reused.

【0021】[0021]

【発明の効果】以上のように、請求項1記載の脆性成形
体によれば、多量の純鉄を含むものであるので、例えば
粉状に加工することによって、高品質の製鋼原料用ブリ
ケットや焼結金属の材料等として再利用が可能であり、
環境保全に役立つとともに研削切粉の廃棄コストを削減
することができる。請求項2記載の脆性成形体によれ
ば、固形化補助剤で固形化しているので、これを所望の
強度にすることができる。このため、崩壊し難く、運
搬、貯蔵等の取り扱いが容易なものになる。
As described above, according to the brittle compact according to the first aspect, since it contains a large amount of pure iron, it can be processed into a powdery form, for example, to produce high quality briquettes for steelmaking raw materials and sintering. It can be reused as metal material, etc.
It is useful for environmental conservation and can reduce the cost of discarding grinding chips. According to the brittle molding according to the second aspect, since it is solidified by the solidification aid, it can have a desired strength. For this reason, it is difficult to disintegrate, and handling such as transportation and storage becomes easy.

【0022】請求項3記載の脆性成形体によれば、前記
固形化補助剤が、コロイダルシリカ、珪酸ソーダ、燐酸
アルミニウム、アスファルト乳剤から選択される少なく
とも1種であるので、油分を含むにもかかわらず強固に
固形化されたものになる。このため、より崩壊し難く、
運搬、貯蔵等の取り扱いがさらに容易なものになる。請
求項4記載の脆性成形体によれば、含油率が1〜5重量
%であるので、適度の硬さに固形化されているととも
に、最小限の残留油分によって研削切粉の成分である純
鉄が酸化するのを効果的に防止することができる。
According to the brittle molding according to the third aspect, since the solidification aid is at least one selected from colloidal silica, sodium silicate, aluminum phosphate, and asphalt emulsion, it contains oil. It becomes a solid that has been solidified. For this reason, it is harder to collapse,
Handling such as transportation and storage becomes easier. According to the brittle molded product according to the fourth aspect, since the oil content is 1 to 5% by weight, it is solidified to an appropriate hardness, and is a component of the ground swarf with a minimum residual oil content. Oxidation of iron can be effectively prevented.

【0023】請求項5記載の脆性成形体の製造方法によ
れば、前記綿状凝集体の圧縮成形によって、従来せん断
が困難であった繊維状の研削切粉を容易にせん断するこ
とができる。また、前記圧縮成形を研削液に含まれてい
る油分を保持した状態で行うので、研削切粉の成分であ
る純鉄が酸化するのを防止することができる。このた
め、多量の純鉄を含む脆性成形体を容易且つ確実に得る
ことができる。
According to the method for manufacturing a brittle molded product according to the fifth aspect, the compression molding of the flocculent agglomerates can easily shear the fibrous ground chips which have been difficult to shear in the past. Further, since the compression molding is performed while retaining the oil content contained in the grinding fluid, it is possible to prevent the pure iron, which is a component of the grinding chips, from being oxidized. For this reason, a brittle compact containing a large amount of pure iron can be easily and reliably obtained.

【0024】請求項6記載の脆性成形体の製造方法によ
れば、前記脆性成形体に含浸させた固形化補助剤によっ
て、所望の強度に固形化された脆性成形体を得ることが
できる。このため、崩壊し難く、運搬、貯蔵等の取り扱
いが容易な脆性成形体を得ることができる。請求項7記
載の脆性成形体の製造方法によれば、前記固形化補助剤
として、コロイダルシリカ、珪酸ソーダ、燐酸アルミニ
ウムアスファルト乳剤から選択される少なくとも1種を
用いるので、油分を含むにもかかわらず強固に固形化さ
れた脆性成形体を得ることができる。このため、より崩
壊し難く、運搬、貯蔵等の取り扱いがさらに容易な脆性
成形体を得ることができる。
According to the method for manufacturing a brittle molded product according to the sixth aspect, a brittle molded product solidified to a desired strength can be obtained by the solidification aid impregnated in the brittle molded product. Therefore, it is possible to obtain a brittle molded body that is hardly disintegrated and easy to handle such as transportation and storage. According to the method for producing a brittle molded article according to claim 7, since at least one selected from colloidal silica, sodium silicate, and aluminum phosphate asphalt emulsion is used as the solidification aid, the solidification aid contains oil. A strongly solidified brittle molded body can be obtained. Therefore, it is possible to obtain a brittle molded body that is less likely to collapse and that is easier to handle such as transport and storage.

【0025】請求項8記載の脆性成形体の製造方法によ
れば、前記固形化補助剤を2〜30重量%混合するの
で、より一層強固に固形化された脆性成形体を得ること
ができる。このため、より一層崩壊し難く、運搬、貯蔵
等の取り扱いがきわめて容易な脆性成形体を得ることが
できる。請求項9記載の脆性成形体の製造方法によれ
ば、前記綿状凝集体として含水率が50重量%を超えな
い範囲に、含油率が10重量%を超えない範囲にそれぞ
れ調整したものを用いるので、前記綿状凝集体の運搬等
の取り扱いが容易となるとともに、圧縮成形のみによっ
て脆性成形体の余剰の水分及び油分を容易かつ適正に除
去することができる。
According to the method for producing a brittle molded product according to the eighth aspect, since the solidification aid is mixed in an amount of 2 to 30% by weight, a brittle molded product which is more solidified can be obtained. For this reason, it is possible to obtain a brittle molded body that is more difficult to collapse and that is extremely easy to handle such as transportation and storage. According to the method for producing a brittle molded product according to the ninth aspect, the flocculent aggregate is used in which the water content is adjusted to a range not exceeding 50% by weight and the oil content is adjusted to a range not exceeding 10% by weight. Therefore, handling such as transportation of the flocculent aggregate is facilitated, and excess moisture and oil content of the brittle molded body can be easily and appropriately removed only by compression molding.

【0026】請求項10記載の脆性成形体の製造方法に
よれば、前記脆性成形体の含水率を2〜12重量%、含
油率を1〜5重量%に調整するので、脆性成形体を適度
の硬さに固形化することができるとともに、最小限の残
留油分によって研削切粉の成分である純鉄が酸化するの
を効果的に防止することができる。請求項11記載の脆
性成形体の製造方法によれば、スプリングバックの大き
い炭素を0.2重量%以上含む研削切粉についても、そ
のスプリングバックの影響を排除して前記圧縮成形によ
り効果的にせん断することができる。
According to the method for manufacturing a brittle molded product according to the tenth aspect, the water content of the brittle molded product is adjusted to 2 to 12% by weight and the oil content is adjusted to 1 to 5% by weight. , And the oxidation of pure iron, which is a component of the ground swarf, can be effectively prevented by the minimum residual oil content. According to the method for manufacturing a brittle molded product according to the eleventh aspect, even with respect to ground chips containing 0.2% by weight or more of carbon having a large springback, the influence of the springback is eliminated and the compression molding is effectively performed. Can be sheared.

【図面の簡単な説明】[Brief description of the drawings]

【図1】この発明の一実施形態に係る脆性成形体の製造
方法を示す工程図である。
FIG. 1 is a process chart showing a method for producing a brittle molded body according to one embodiment of the present invention.

【図2】脆性成形体からブリケットを製造する方法を示
す工程図である。
FIG. 2 is a process chart showing a method for producing briquettes from brittle molded bodies.

【図3】脆性成形体からブリケットを製造する他の方法
を示す工程図である。
FIG. 3 is a process chart showing another method for producing briquettes from brittle moldings.

【図4】脆性成形体の他の形状を示す一部欠截斜視図で
ある。
FIG. 4 is a partially cutaway perspective view showing another shape of the brittle molded body.

【符号の説明】[Explanation of symbols]

A 脆性成形体 B 綿状凝集体 C 脆性成形体 D 固形化補助剤 E 粉体 G ブリケット A Brittle molded body B Cotton-like aggregate C Brittle molded body D Solidification aid E Powder G Briquette

───────────────────────────────────────────────────── フロントページの続き (72)発明者 松田 光馬 大阪市中央区南船場三丁目5番8号 光洋 精工株式会社内 (72)発明者 清尾 良弘 大阪市中央区南船場三丁目5番8号 光洋 精工株式会社内 (72)発明者 樫野 彰一 大阪市中央区南船場三丁目5番8号 光洋 精工株式会社内 Fターム(参考) 4K018 AA24 BA14 BB08 CA07 CA11 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Mitsuma Matsuda 3-5-8 Minamisenba, Chuo-ku, Osaka-shi Koyo Seiko Co., Ltd. (72) Yoshihiro Kiyoo 3-58 Minamisenba, Chuo-ku, Osaka-shi Koyo Inside Seiko Co., Ltd. (72) Shoichi Kashino 3-5-8 Minamisenba, Chuo-ku, Osaka-shi Koyo Seiko Co., Ltd. F term (reference) 4K018 AA24 BA14 BB08 CA07 CA11

Claims (11)

【特許請求の範囲】[Claims] 【請求項1】鉄系金属の研削切粉と油分及び水分を含有
する研削液とを含む綿状凝集体を所定形状に圧縮成形し
てなることを特徴とする脆性成形体。
1. A brittle molded product obtained by compression-molding a flocculent aggregate containing iron-based metal ground chips and a grinding fluid containing oil and water into a predetermined shape.
【請求項2】固形化補助剤で固形化してなる請求項1記
載の脆性成形体。
2. The brittle molded article according to claim 1, which is solidified with a solidification aid.
【請求項3】前記固形化補助剤が、コロイダルシリカ、
珪酸ソーダ、燐酸アルミニウム、アスファルト乳剤から
選択される少なくとも1種である請求項1記載の脆性成
形体。
3. The method according to claim 1, wherein the solidification aid is colloidal silica,
The brittle molded product according to claim 1, wherein the brittle molded product is at least one selected from sodium silicate, aluminum phosphate, and asphalt emulsion.
【請求項4】前記脆性成形体の含油率が1〜5重量%で
ある請求項1記載の脆性成形体。
4. The brittle molded article according to claim 1, wherein said brittle molded article has an oil content of 1 to 5% by weight.
【請求項5】鉄系金属の研削切粉と油分及び水分を含有
する研削液とを含む綿状凝集体を圧縮成形して、繊維状
の研削切粉がせん断され且つ余剰の水分及び油分が除去
された所定形状の脆性成形体を得ることを特徴とする脆
性成形体の製造方法。
5. A flocculent agglomerate containing a grinding chip of an iron-based metal and a grinding fluid containing oil and water is compression-molded, whereby the fibrous grinding chips are sheared and excess water and oil are removed. A method for producing a brittle molded product, wherein a brittle molded product having a predetermined shape removed is obtained.
【請求項6】前記脆性成形体に固形化補助剤を含浸させ
る工程をさらに含む請求項5記載の脆性成形体の製造方
法。
6. The method for producing a brittle molded article according to claim 5, further comprising a step of impregnating the brittle molded article with a solidification aid.
【請求項7】前記固形化補助剤として、コロイダルシリ
カ、珪酸ソーダ、燐酸アルミニウム、アスファルト乳剤
から選択される少なくとも1種を用いる請求項6記載の
脆性成形体の製造方法。
7. The method according to claim 6, wherein at least one selected from the group consisting of colloidal silica, sodium silicate, aluminum phosphate, and asphalt emulsion is used as the solidification aid.
【請求項8】前記固形化補助剤を2〜30重量%含浸さ
せる請求項7記載の脆性成形体の製造方法。
8. The method for producing a brittle molded product according to claim 7, wherein the solidification aid is impregnated with 2 to 30% by weight.
【請求項9】前記綿状凝集体として、含水率が50重量
%を超えない範囲に、含油率が10重量%を超えない範
囲にそれぞれ調整したものを用いる請求項5記載の脆性
成形体の製造方法。
9. The brittle molded article according to claim 5, wherein the flocculent aggregate is adjusted to a water content not exceeding 50% by weight and an oil content not exceeding 10% by weight. Production method.
【請求項10】前記脆性成形体の含水率を2〜12重量
%、含油率を1〜5重量%に調整する請求項5記載の脆
性成形体の製造方法。
10. The method for producing a brittle molded article according to claim 5, wherein the moisture content of the brittle molded article is adjusted to 2 to 12% by weight and the oil content is adjusted to 1 to 5% by weight.
【請求項11】前記研削切粉として、炭素を0.2重量
%以上含むものを用いる請求項5記載の脆性成形体の製
造方法。
11. The method for producing a brittle molded product according to claim 5, wherein a material containing 0.2% by weight or more of carbon is used as said ground swarf.
JP2001302116A 2000-10-02 2001-09-28 Powder for solid material and method for producing the same Expired - Lifetime JP3774652B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2001302116A JP3774652B2 (en) 2000-10-02 2001-09-28 Powder for solid material and method for producing the same

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2000-302339 2000-10-02
JP2000302339 2000-10-02
JP2001302116A JP3774652B2 (en) 2000-10-02 2001-09-28 Powder for solid material and method for producing the same

Publications (2)

Publication Number Publication Date
JP2002180108A true JP2002180108A (en) 2002-06-26
JP3774652B2 JP3774652B2 (en) 2006-05-17

Family

ID=26601365

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2001302116A Expired - Lifetime JP3774652B2 (en) 2000-10-02 2001-09-28 Powder for solid material and method for producing the same

Country Status (1)

Country Link
JP (1) JP3774652B2 (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005240087A (en) * 2004-02-25 2005-09-08 Koyo Seiko Co Ltd Briquette for raw material for steelmaking and method for manufacturing the same
JP2005256116A (en) * 2004-03-12 2005-09-22 Koyo Seiko Co Ltd Briquette for metal raw material and its producing method
JP2005256051A (en) * 2004-03-10 2005-09-22 Koyo Seiko Co Ltd Briquette for steelmaking raw material and its producing method
JP2005298946A (en) * 2004-04-15 2005-10-27 Koyo Seiko Co Ltd Method for producing briquette for metal raw material
JP2006265617A (en) * 2005-03-23 2006-10-05 Nisshin Steel Co Ltd Method of producing scrap wood briquette for refining furnace and scrap wood briquette for refining furnace produced by the method
WO2014127083A1 (en) * 2013-02-14 2014-08-21 Baker Hughes Incorporated Colloidal silica addition to promote the separation of oil from water

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005240087A (en) * 2004-02-25 2005-09-08 Koyo Seiko Co Ltd Briquette for raw material for steelmaking and method for manufacturing the same
JP2005256051A (en) * 2004-03-10 2005-09-22 Koyo Seiko Co Ltd Briquette for steelmaking raw material and its producing method
JP2005256116A (en) * 2004-03-12 2005-09-22 Koyo Seiko Co Ltd Briquette for metal raw material and its producing method
JP2005298946A (en) * 2004-04-15 2005-10-27 Koyo Seiko Co Ltd Method for producing briquette for metal raw material
JP4710242B2 (en) * 2004-04-15 2011-06-29 株式会社ジェイテクト Method for producing briquettes for metal raw materials
JP2006265617A (en) * 2005-03-23 2006-10-05 Nisshin Steel Co Ltd Method of producing scrap wood briquette for refining furnace and scrap wood briquette for refining furnace produced by the method
WO2014127083A1 (en) * 2013-02-14 2014-08-21 Baker Hughes Incorporated Colloidal silica addition to promote the separation of oil from water

Also Published As

Publication number Publication date
JP3774652B2 (en) 2006-05-17

Similar Documents

Publication Publication Date Title
KR100624295B1 (en) Briquette as material for steel making and method for production thereof
US7135053B2 (en) Brittle formed product and iron-based power material and method for manufacturing these materials
US20080179788A1 (en) Method of Forming a Briquette
JP3746978B2 (en) Manufacturing method of briquette for steelmaking raw material
JP2008163412A (en) Ferrous powder material, its production method, and briquette for raw material for steel making
JP3774652B2 (en) Powder for solid material and method for producing the same
JP3711046B2 (en) Manufacturing method of briquette for steelmaking raw material
JP3711045B2 (en) Briquette for steelmaking raw materials
JP3745657B2 (en) Manufacturing method of briquette for steelmaking raw material
JP3789796B2 (en) Iron-based powder material and manufacturing method thereof
JP2004269960A (en) Briquette for raw material in steelmaking
EP1454996B1 (en) Briquette for raw material for iron manufacture and briquette for introduction into slag generating apparatus
JP2005126826A (en) Method for manufacturing briquette of raw steelmaking material
JP2005240087A (en) Briquette for raw material for steelmaking and method for manufacturing the same
JP2005163187A (en) Briquette as raw material for steel making
WO2005080614A1 (en) Briquette as steelmaking raw material and process for producing the same
JP3701945B2 (en) Briquette for slag generator
JP2005187946A (en) Brittle compact and briquette using it

Legal Events

Date Code Title Description
A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20040301

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A132

Effective date: 20051101

A521 Written amendment

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20051222

TRDD Decision of grant or rejection written
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20060120

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20060220

R150 Certificate of patent or registration of utility model

Ref document number: 3774652

Country of ref document: JP

Free format text: JAPANESE INTERMEDIATE CODE: R150

Free format text: JAPANESE INTERMEDIATE CODE: R150

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20100224

Year of fee payment: 4

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20100224

Year of fee payment: 4

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20110224

Year of fee payment: 5

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20110224

Year of fee payment: 5

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20120224

Year of fee payment: 6

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20120224

Year of fee payment: 6

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20130224

Year of fee payment: 7

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20130224

Year of fee payment: 7

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20140224

Year of fee payment: 8

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250