JP2882838B2 - Surface-treated needle-like or whisker-like aragonite calcium carbonate and polypropylene-based resin composition containing the calcium carbonate - Google Patents
Surface-treated needle-like or whisker-like aragonite calcium carbonate and polypropylene-based resin composition containing the calcium carbonateInfo
- Publication number
- JP2882838B2 JP2882838B2 JP4421290A JP4421290A JP2882838B2 JP 2882838 B2 JP2882838 B2 JP 2882838B2 JP 4421290 A JP4421290 A JP 4421290A JP 4421290 A JP4421290 A JP 4421290A JP 2882838 B2 JP2882838 B2 JP 2882838B2
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- whisker
- calcium carbonate
- aragonite
- weight
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Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は表面処理針状又はウイスカー状アラゴナイト
炭酸カルシウム（以下、ウイスカー状アラゴナイト炭カ
ルと略記する。また、以下、炭酸カルシウムを炭カルと
略記する。）に関し、更に詳しくは、長径10〜100μ
ｍ、短径0.5〜4.0μｍのウイスカー状アラゴナイト炭カ
ルを石油樹脂で表面処理することによって、特にポリプ
ロピレン系樹脂（以下、PPと略記する）に配合した場合
に優れた剛性を付与することができる表面処理ウイスカ
ー状アラゴナイト炭カルに関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a surface-treated needle-like or whisker-like aragonite calcium carbonate (hereinafter abbreviated as whisker-like aragonite charcoal. In the following, calcium carbonate is abbreviated as carbon calcium). More specifically, the major axis 10 ~ 100μ
m, whisker-like aragonite char having a minor axis of 0.5 to 4.0 μm can be provided with excellent rigidity by surface-treating the aragonite char with a petroleum resin, particularly when blended with a polypropylene resin (hereinafter abbreviated as PP). The present invention relates to a surface-treated whisker-like aragonite char.
PPは、その用途によっては剛性が不足するため、各種
無機物を配合することによって剛性を向上させている。
無機物としては、タルク、ガラス繊維、ウォラストナイ
ト、炭カル等が用いられている。しかし、これらは一長
一短があり、PP用配合物としては十分に満足できるもの
ではない。具体的には、タルクは天然物であるため白度
が悪く、また盤状という形状に起因していると考えられ
るウエルド面での強度が悪い。ガラス繊維は優れた剛性
を発揮するが、粗大粒子のためPP成形品の表面平滑性が
悪く、且つ射出成形時の流れも悪い。ウォラストナイト
はタルク同様天然物のため白度が悪く、且つガラス繊維
と同様の表面の平滑性に問題がある。最後に、炭カルは
上記のような問題はないが、主目的の剛性が不十分であ
る。これは、現在、汎用的に使用されている炭カルの形
状が不定形、立方体、紡錘形であることに起因する。こ
の形状を変えることによって、即ち、針状又はウイスカ
ー状にすることによって、この問題の解決を図ろうとす
る技術が提案されている。例えば、特開平１−278566、
特開平１−234437、特開平１−163221等がある。Rigidity of PP is insufficient depending on its application, and thus the rigidity is improved by blending various inorganic substances.
As the inorganic substance, talc, glass fiber, wollastonite, charcoal and the like are used. However, these have advantages and disadvantages and are not sufficiently satisfactory as a blend for PP. Specifically, since talc is a natural product, its whiteness is poor, and its strength on the weld surface, which is considered to be caused by a disk-like shape, is poor. Glass fibers exhibit excellent rigidity, but due to coarse particles, the surface smoothness of PP molded products is poor, and the flow during injection molding is also poor. Wollastonite, like talc, is a natural product and therefore has poor whiteness, and has a problem in surface smoothness similar to glass fibers. Finally, charcoal does not have the above problems, but has insufficient rigidity for the main purpose. This is attributable to the fact that the shape of charcoal commonly used at present is irregular, cubic, or spindle-shaped. Techniques have been proposed that attempt to solve this problem by changing this shape, that is, by making it needle-like or whisker-like. For example, JP-A-1-278566,
There are JP-A-1-234437 and JP-A-1-163221.
従来からアスペクト比の大きい針状又はウイスカー状
炭カル（以下、ウイスカー状炭カルと記す）が開発され
れば、天然物のもつ欠点を克服し、優れた剛性が発揮さ
れるであろうと考えられていた。これらについての知見
は10年以上も前から刊行物に記載され公知の事実となっ
ている。It is thought that if needle-like or whisker-like coal cal having a large aspect ratio (hereinafter, referred to as whisker-like coal cal) is developed, the disadvantages of natural products will be overcome and excellent rigidity will be exhibited. I was These findings have been described in publications for more than 10 years and are known facts.
しかし乍ら、最近に至るまでアスペクト比の大きなウ
イスカー状炭カル（長径20μｍ以上）の工業的に容易に
得るための生成技術がなかったため、PPでの効果を確認
できなかったのが実情である。However, until recently, there was no production technology for industrially easily obtaining whisker-like carbon (having a major axis of 20 μm or more) having a large aspect ratio, so that the effect of PP could not be confirmed. .
本発明者らはかかる実情の中で、アスペクト比の大き
いウイスカー状アラゴナイト炭カルを工業的に容易に得
るための製造方法を確立し、先に特願平１−167267号
（特開平３−88714号）として出願済みである。しかし
乍ら、その後も引き続いて研究する過程で、ウイスカー
状アラゴナイト炭カルの場合、その効果をより一層発揮
させるためには、その表面を処理してPPとなじみの良い
状態に改質する必要がある。これらの表面処理をしない
と、後記比較応用例１に示すように、たとえ形状が針状
であれ、ウイスカー状であれ、その形状効果を最大限に
発揮させることができない。これはPPとこれら無機物と
の相溶性が悪いと、力が加わった時に両者が容易に剥離
し、十分な剛性を発揮することができないためである。Under such circumstances, the present inventors have established a production method for industrially easily obtaining whisker-like aragonite coal having a large aspect ratio, and have previously described Japanese Patent Application No. 1-167267 (Japanese Patent Application Laid-Open No. 3-88714). No.). However, in the course of subsequent research, in the case of whisker-like aragonite char, it is necessary to treat the surface of the whisker-like aragonite char to improve its effect so that the surface is compatible with PP. is there. Without these surface treatments, as shown in Comparative Application Example 1 below, the shape effect cannot be maximized even if the shape is needle-like or whisker-like. This is because if the compatibility between PP and these inorganic substances is poor, they are easily peeled off when a force is applied, so that sufficient rigidity cannot be exhibited.
本発明者らはかかる実情に鑑み鋭意研究の結果、ウイ
スカー状アラゴナイト炭カルに石油樹脂をコーティング
することによって、その形状効果を最大限に発揮させ得
ることを見出し、本発明を完成させるに至った。The present inventors have conducted intensive studies in view of such circumstances, and as a result, have found that by coating a whisker-like aragonite charcoal with a petroleum resin, the shape effect can be maximized, and have completed the present invention. .
即ち、本発明の第１は、長径10〜100μｍ、短径0.5〜
4.0μｍの針状又はウイスカー状アラゴナイト炭酸カル
に石油樹脂を表面処理してなる表面処理ウイスカー状ア
ラゴナイト炭酸カルを、 本発明の第２は、前記表面処理ウイスカー状アラゴナ
イト炭酸カルをポリプロピレン系樹脂100重量部に対し
て５〜50重量部配合してなるポリプロピレン系樹脂組成
物をそれぞれ内容とするものである。That is, the first aspect of the present invention is that the major axis is 10 to 100 μm and the minor axis is 0.5 to 100 μm.
A surface-treated whisker-like aragonite carbonate obtained by surface-treating a petroleum resin on 4.0 μm needle-like or whisker-like aragonite carbonate, The second of the present invention is that the surface-treated whisker-like aragonite carbonate is 100% by weight of a polypropylene resin. The content of the polypropylene resin composition is from 5 to 50 parts by weight per part.
本発明に用いられるウイスカー状アラゴナイト炭カル
は、長径10〜100μｍ、短径0.5〜4.0μｍである。この
炭カルの作り方としては例えば、特願平１−167267（特
願平３−88714号）に詳細に説明されている。具体的に
は、Ca（OH）２の水スラリーにCO2ガスを吹き込んで炭
酸カルシウムを生成させるに際し、アラゴナイト結晶炭
酸カルとCa（OH）２のモル比が1:7〜1:100になる割合で
予め混合した水スラリーを作り、これに可溶性リン酸化
合物を添加してCO2ガスにより炭酸化させる。The whisker-like aragonite coal used in the present invention has a major axis of 10 to 100 μm and a minor axis of 0.5 to 4.0 μm. The method of making the char is described in detail in, for example, Japanese Patent Application No. 1-167267 (Japanese Patent Application No. 3-88714). Specifically, when a CO 2 gas is blown into a water slurry of Ca (OH) 2 to generate calcium carbonate, the molar ratio of aragonite crystal calcium carbonate to Ca (OH) 2 becomes 1: 7 to 1: 100. A premixed water slurry is prepared, to which a soluble phosphoric acid compound is added and carbonized by CO 2 gas.
上記アラゴナイト炭カルはモル比で1:7〜1:100、好ま
しくは1:10〜1:100、より好ましくは1:15〜1:100の割合
となるように混合される。モル比が1:7未満では本発明
の目的とする大粒子のものが得られ難く、また1:100を
越えると、やはり微細な粒子となる。アラゴナイト炭カ
ルとCa（OH）２混合スラリーの濃度は30〜250g/が好
ましく、より好ましくは100〜230g/である。The aragonite char is mixed in a molar ratio of 1: 7 to 1: 100, preferably 1:10 to 1: 100, more preferably 1:15 to 1: 100. If the molar ratio is less than 1: 7, it is difficult to obtain large particles as the object of the present invention, and if it exceeds 1: 100, fine particles are also obtained. The concentration of the mixed slurry of aragonite char and Ca (OH) 2 is preferably 30 to 250 g /, more preferably 100 to 230 g /.
用いられる可溶性リン酸化合物としては、リン酸及び
リン酸のNa塩、Ｋ塩、NH4塩等が挙げられ、これらは単
独又は２種以上混合して用いられる。これらリン酸の塩
としては、K3PO4,KH2PO4,K2HPO4,NA2HPO4・12H2O,（N
H4）3PO4,・3H2O等が例示される。可溶性の程度につい
ては0.1g/100cc（20℃の水）以上、好ましくは5.0g/100
cc（20℃の水）以上水に溶けるものが良い。可溶性リン
酸化合物の添加量はCa（OH）２に対して0.1〜15重量％
が好ましく、より好ましくは0.3〜5.0重量％である。Examples of the soluble phosphoric acid compound to be used include phosphoric acid and Na salt, K salt, NH 4 salt of phosphoric acid, and these may be used alone or in combination of two or more. These phosphoric acid salts include K 3 PO 4 , KH 2 PO 4 , K 2 HPO 4 , NA 2 HPO 4 and 12H 2 O, (N
H 4 ) 3 PO 4 , .3H 2 O and the like. 0.1g / 100cc (20 ° C water) or more, preferably 5.0g / 100
It should be soluble in water at least cc (20 ℃ water). The amount of the soluble phosphate compound added is 0.1 to 15% by weight based on Ca (OH) 2 .
Is more preferable, and more preferably 0.3 to 5.0% by weight.
炭酸化は20〜80℃が好ましく、より好ましくは40〜80
℃である。またCO2ガス導入量はCO2100％として４/mi
n/kg・Ca（OH）２以下が好ましく、より好ましくは２
/min/kg・Ca（OH）２である。Carbonation is preferably 20-80 ° C, more preferably 40-80 ° C.
° C. The amount of CO 2 gas introduced is 4 / mi assuming 100% CO 2
n / kg · Ca (OH) 2 or less is preferable, and 2 is more preferable.
/ min / kg · Ca (OH) 2 .
上記の如くして得られた長径10〜100μｍ、短径0.5〜
4.0μｍのウイスカー状アラゴナイト炭カルは、この形
状効果のために、PPに配合した場合、相当な剛性を付与
することができる。しかし乍ら、炭カル表面は親水性で
あるため、疎水性であるPPとの相溶性は良くない。両者
の相溶性が良くないと、力が加わった際に両者の密着力
が十分でないため、PPと炭カルが容易に剥離してしま
う。このため、ウイスカー状という形状効果を最大限に
発揮することができない。この問題を解決するために、
ウイスカー状アラゴナイト炭カルの表面を石油樹脂でコ
ーティングする。この表面処理により両者の相溶性が向
上し、且つウイスカー状アラゴナイト炭カルの剛性が一
層向上し、該表面処理ウイスカー状アラゴナイト炭カル
を配合したPPの剛性が尚一層向上する。The major axis obtained as described above is 10 to 100 μm, and the minor axis is 0.5 to
Due to this shape effect, whisker-like aragonite char of 4.0 μm can impart considerable rigidity when blended with PP. However, since the surface of the carbonaceous material is hydrophilic, its compatibility with the hydrophobic PP is not good. If the compatibility between the two is not good, when the force is applied, the adhesion between the two is not sufficient, so that the PP and the coal are easily separated. Therefore, the whisker-like shape effect cannot be maximized. to solve this problem,
The surface of whisker-like aragonite char is coated with petroleum resin. By this surface treatment, the compatibility of both is improved, and the rigidity of the whisker-like aragonite char is further improved, and the rigidity of the PP containing the surface-treated whisker-like aragonite char is further improved.
表面処理剤として使用する石油樹脂とは、石油精製工
程中等で得られる特定留分中の重合可能な物質を単離精
製することなしにそのまま重合し、樹脂化したものであ
る。The petroleum resin used as the surface treatment agent is obtained by polymerizing a polymerizable substance in a specific fraction obtained in a petroleum refining process or the like without isolating and purifying the same, and converting it into a resin.
表面処理の方法としては湿式でも乾式でもよいが、ウ
イスカー状アラゴナイト炭カルの生成工程から考えて湿
式の方が好ましい。湿式で表面処理する場合は、石油樹
脂は水等に可溶性の状態にする必要がある。石油樹脂は
本来不溶性であるので、これを可溶性にするためにはカ
ルボキシル基等の親水基をグラフトさせる。具体的には
マレイン酸等でマレイン化する方法が好ましい。こうし
て親水基をグラフトしても、通常は十分な可溶状態とは
ならず、そこでロジン等の界面活性剤を使用してエマル
ジョン化するのが一般的である。この状態のものをウイ
スカー状アラゴナイト炭カルの水スラリーに投入し十分
撹拌した後、脱水、乾燥して粉体化すればよい。この場
合のウイスカー状アラゴナイト炭カルスラリーの濃度
は、生成工程から考えて炭カル30g/〜200g/程度が
好ましい。石油樹脂の表面処理量は固形分で炭カルに対
して0.1〜10重量％、好ましくは0.5〜３重量％がよい。
一方乾式で表面処理する場合は石油樹脂の固形分をウイ
スカー状アラゴナイト炭カル粉体と共にヘンシェルミキ
サー等で混合撹拌すればよい。表面処理量等は湿式と同
程度でよい。The method of surface treatment may be a wet method or a dry method, but the wet method is more preferable in view of the whisker-like aragonite char formation process. When the surface treatment is performed by a wet method, the petroleum resin needs to be in a state of being soluble in water or the like. Since a petroleum resin is essentially insoluble, a hydrophilic group such as a carboxyl group is grafted to make it soluble. Specifically, a method of maleating with maleic acid or the like is preferable. Even if a hydrophilic group is grafted in this way, it usually does not become a sufficiently soluble state, and thus it is general to emulsify using a surfactant such as rosin. In this state, whisker-like aragonite char is added to a water slurry, stirred sufficiently, and then dewatered and dried to form a powder. In this case, the concentration of the whisker-like aragonite coal slurry is preferably about 30 g / -200 g / carbon, considering the production process. The surface treatment amount of the petroleum resin is 0.1 to 10% by weight, preferably 0.5 to 3% by weight, based on the solid carbon content of the petroleum resin.
On the other hand, when the surface treatment is performed by a dry method, the solid content of the petroleum resin may be mixed and stirred with a whisker-like aragonite carbon powder using a Henschel mixer or the like. The surface treatment amount and the like may be about the same as the wet type.
上記の如くして得られた表面処理ウイスカー状アラゴ
ナイト炭カルは、PP100重量部に対して５〜50重量部、
好ましくは20〜30重量部配合される。The surface-treated whisker-like aragonite char obtained as described above is 5 to 50 parts by weight with respect to 100 parts by weight of PP.
Preferably, 20 to 30 parts by weight are blended.
以下、実施例に基づいて本発明を更に詳細に説明する
が、本発明はこれらにのみ限定されるものではない。Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited thereto.
実施例１ 特願平１−167267号（特願平３−88714号）の方法で
平均長径40μｍ、平均短径1.7μｍのウイスカー状アラ
ゴナイト炭カルを生成させ、生成直後の水スラリーの濃
度が炭カル150g/になるように調整した。Example 1 Whisker-like aragonite coal having an average major axis of 40 μm and an average minor axis of 1.7 μm was produced by the method of Japanese Patent Application No. 1-167267 (Japanese Patent Application No. 3-88714). It was adjusted to 150 g / cal.
このスラリーに石油樹脂を炭カルに対して2.0重量％
添加して表面処理した。この石油樹脂は石油樹脂／ロジ
ン＝3/1の比率でエマルジョン化したもので、固形分濃
度は40重量％であった。こうして表面処理したウイスカ
ー状アラゴナイト炭カルを脱水、乾燥して粉体化した。2.0% by weight of petroleum resin to charcoal in this slurry
It was added and surface-treated. This petroleum resin was emulsified in a ratio of petroleum resin / rosin = 3/1, and had a solid content of 40% by weight. The surface-treated whisker-like aragonite char was dehydrated, dried and powdered.
比較例１ 石油樹脂で表面処理をしないこと以外は全て実施例１
と同様の方法でウイスカー状アラゴナイト炭カルを作
り、粉体化した。Comparative Example 1 Example 1 except that no surface treatment was performed with petroleum resin.
Whisker-like aragonite char was prepared and powdered in the same manner as described above.
応用例、比較応用例１〜２ 実施例１、比較例１で生成したウイスカー炭カル、一
般にPP用フィラーとして広く使用されているタルク（富
士タルク製、PKS−100）を用いて、下記の要領でポリプ
ロピレンに配合し強度物性を測定した。Application Examples, Comparative Application Examples 1-2 Using the whisker coal calc produced in Example 1 and Comparative Example 1 and talc (PKS-100, manufactured by Fuji Talc), which is widely used as a filler for PP in general, the following procedure And blended with polypropylene to measure the strength properties.
（１）試験法 配合： ポリプロピレン樹脂（商品名MA−３、三菱油化製） 100重量部 試料 30重量部 この配合比で混練してペレット化した後、射出成型し
て試験片を作り強度物性を測定した。結果を第１表に示
した。(1) Test method Compounding: 100 parts by weight of polypropylene resin (trade name: MA-3, manufactured by Mitsubishi Yuka) 30 parts by weight of sample Kneading at this mixing ratio, pelletizing, injection molding to form a test piece, and strength properties Was measured. The results are shown in Table 1.
第１表の結果より、本発明品はPPに配合した場合、優
れた強度物性を発揮することが判る。 From the results shown in Table 1, it can be seen that the product of the present invention exhibits excellent strength properties when blended with PP.
本発明の表面処理ウイスカー状アラゴナイト炭カルは
PPとの相溶性が改善されているため、その形状効果を一
層効果的に発揮し、PPの剛性を顕著に向上させる。ま
た、本発明の表面処理ウイスカー状アラゴナイト炭カル
は、PPと同様の剛性や相溶性に問題のある他の合成樹脂
等に対する充填剤としても利用できることは言うまでも
ない。The surface-treated whisker-like aragonite char of the present invention is
Since the compatibility with PP is improved, the shape effect is more effectively exhibited, and the rigidity of PP is significantly improved. In addition, it goes without saying that the surface-treated whisker-like aragonite char of the present invention can also be used as a filler for other synthetic resins or the like that have the same problems of rigidity and compatibility as PP.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.6，ＤＢ名) C09C 1/00 - 3/12 C08K 3/00 - 13/08 ──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int. Cl. 6 , DB name) C09C 1/00-3/12 C08K 3/00-13/08
Claims (5)
状又はウイスカー状アラゴナイト炭酸カルシウム（以
下、ウイスカー状アラゴナイト炭酸カルシウムと記す）
に石油樹脂を表面処理してなる表面処理ウイスカー状ア
ラゴナイト炭酸カルシウム。An acicular or whisker-like aragonite calcium carbonate having a major axis of 10 to 100 μm and a minor axis of 0.5 to 4.0 μm (hereinafter referred to as whisker-like aragonite calcium carbonate).
Surface-treated whisker-like aragonite calcium carbonate obtained by subjecting petroleum resin to surface treatment.
ゴナイト炭酸カルシウムに対して0.1〜10重量％である
請求項１記載の表面処理炭酸カルシウム。2. The surface-treated calcium carbonate according to claim 1, wherein the surface treatment amount of the petroleum resin is 0.1 to 10% by weight based on the whisker-like aragonite calcium carbonate.
ゴナイト炭酸カルシウムに対して0.5〜３重量％である
請求項１記載の表面処理炭酸カルシウム。3. The surface-treated calcium carbonate according to claim 1, wherein the surface treatment amount of the petroleum resin is 0.5 to 3% by weight based on the whisker-like aragonite calcium carbonate.
カー状アラゴナイト炭酸カルシウムをポリプロピレン系
樹脂100重量部に対して５〜50重量部配合してなるポリ
プロピレン系樹脂組成物。4. A polypropylene resin composition comprising the surface-treated whisker-like aragonite calcium carbonate according to any one of claims 1 to 3 in an amount of 5 to 50 parts by weight per 100 parts by weight of the polypropylene resin.
ルシウムをポリプロピレン系樹脂100重量部に対して20
〜30重量部配合してなる請求項４記載の樹脂組成物。5. A whisker-like aragonite calcium carbonate having a surface treatment of 20 parts by weight per 100 parts by weight of a polypropylene resin.
The resin composition according to claim 4, which is blended in an amount of 30 parts by weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4421290A JP2882838B2 (en) | 1990-02-23 | 1990-02-23 | Surface-treated needle-like or whisker-like aragonite calcium carbonate and polypropylene-based resin composition containing the calcium carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4421290A JP2882838B2 (en) | 1990-02-23 | 1990-02-23 | Surface-treated needle-like or whisker-like aragonite calcium carbonate and polypropylene-based resin composition containing the calcium carbonate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03247668A JPH03247668A (en) | 1991-11-05 |
| JP2882838B2 true JP2882838B2 (en) | 1999-04-12 |
Family
ID=12685246
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4421290A Expired - Fee Related JP2882838B2 (en) | 1990-02-23 | 1990-02-23 | Surface-treated needle-like or whisker-like aragonite calcium carbonate and polypropylene-based resin composition containing the calcium carbonate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2882838B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2790765B2 (en) * | 1993-06-17 | 1998-08-27 | 丸尾カルシウム株式会社 | Seal member |
| JP2002309125A (en) * | 2001-04-17 | 2002-10-23 | Maruo Calcium Co Ltd | Inorganic filler for regulating curing characteristics and resin composition formed by blending the same |
-
1990
- 1990-02-23 JP JP4421290A patent/JP2882838B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03247668A (en) | 1991-11-05 |
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| Date | Code | Title | Description |
|---|---|---|---|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
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| LAPS | Cancellation because of no payment of annual fees |