JP3635806B2 - Manufacturing method of mineral fiberboard - Google Patents

Manufacturing method of mineral fiberboard Download PDF

Info

Publication number
JP3635806B2
JP3635806B2 JP24100796A JP24100796A JP3635806B2 JP 3635806 B2 JP3635806 B2 JP 3635806B2 JP 24100796 A JP24100796 A JP 24100796A JP 24100796 A JP24100796 A JP 24100796A JP 3635806 B2 JP3635806 B2 JP 3635806B2
Authority
JP
Japan
Prior art keywords
fine particles
expansion
thermally expandable
weight
mineral
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
Application number
JP24100796A
Other languages
Japanese (ja)
Other versions
JPH1072799A (en
Inventor
一功 小池
英俊 小島
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.)
Nitto Boseki Co Ltd
Original Assignee
Nitto Boseki 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 Nitto Boseki Co Ltd filed Critical Nitto Boseki Co Ltd
Priority to JP24100796A priority Critical patent/JP3635806B2/en
Priority to US08/916,360 priority patent/US5800676A/en
Priority to KR1019970040693A priority patent/KR100245484B1/en
Priority to CNB971176892A priority patent/CN1148506C/en
Publication of JPH1072799A publication Critical patent/JPH1072799A/en
Application granted granted Critical
Publication of JP3635806B2 publication Critical patent/JP3635806B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Landscapes

  • Paper (AREA)
  • Building Environments (AREA)
  • Panels For Use In Building Construction (AREA)

Description

【0001】
【産業上の利用分野】
本発明は、鉱滓綿等の鉱物繊維を主成分とする軽量性、吸音性、生産性に優れ、かつ自然な凹凸模様を機械加工せずに付与できる鉱物質繊維板の湿式製造方法に関する。
【0002】
【従来の技術】
鉱滓綿を主成分とする湿式製造方法による鉱物質繊維板はその防火性能、吸音性能、意匠を特徴として、天井内装材に使われている。しかし従来の鉱物質繊維板はさらなる吸音性の向上及び軽量化が要求されている。また湿式製造方法による成型板の従来の意匠付与方法はロールエンボス、ロールフィッシャー、ロールプレス、サンドブラスト立体加工等があるがいずれも機械設備が必要であるため生産性において意匠付与工程が律速になる。模様に付いては機械によるものであるため人工的、規則的なものになり、自然な感じが得られない。またロールやサンドブラストによる模様は表層だけに施されているためキューブ等の立体加工を併用した場合は谷部に模様を残すことができない。素材全層にわたって模様を残すことは実際上湿式製造方法では不可能であった。
【0003】
【発明が解決しようとする課題】
本発明は鉱物質繊維板の前記潜在的課題を経済的に解決し、軽量性、吸音性、生産性に優れ、かつ自然な凹凸模様を機械加工せずに付与できる鉱物質繊維板の湿式製造方法を提供することにある。
【0004】
【課題を解決するための手段】
前記課題は、鉱物質繊維60〜90重量%、有機結合剤2〜19重量%、無機質微繊維1〜20重量%、凝集剤0.5〜3重量%、膨張後の直径が1.0〜3.0mmであり、直径の膨張倍率が3倍以上であり、かつ膨張開始温度が50〜105℃である熱膨張性微粒子0.5〜7重量%を組成成分とし水中に均一に分散してスラリーとし、次に抄造工程を経てマット状に裁断され、続いて乾燥工程において該マット中の熱膨張性微粒子は加熱され膨張し、有機結合剤の硬化セッティングされる前に熱膨張性微粒子の膨張を終わらせ、次いで有機結合剤の硬化セッティング後に膨張した熱膨張性微粒子を溶融破泡させ、全層に亘って虫喰模様状態を生じさせることを特徴とする鉱物質繊維板の製造方法によって解決される。
【0005】
【発明の実施の形態】
本発明にかかる鉱物質繊維は鉱滓綿、ロックウール等であり使用量は60〜90重量%である。
【0006】
本発明にかかる有機結合剤は樹脂、デンプン、叩解パルプ等で鉱物質繊維等の成分を結合するために2〜19重量%使用される。2重量%より少ないと鉱物質繊維を結合する力が不足し鉱物質繊維板の強度維持に問題が生じ、有機成分の合計が20重量%を越えると、防火性能において準不燃をクリアできなくなるため有機結合剤の上限は19重量%となる。
【0007】
本発明にかかる無機質微繊維はセピオライト、アタパルジャイト等で有機結合剤や熱膨張性樹脂微粒子の歩留り向上材及び自身が固着剤として強度物性の向上に寄与する。使用量は1〜20重量%である。1重量%より少ないと歩留り向上や強度物性の向上の効果が不十分であり、20重量%を越えると主原料の鉱物質繊維の含有量が減少し密度が高くなってしまうことと、抄造工程での濾水性の悪化による生産スピードの低下となり好ましくない。
【0008】
本発明にかかる凝集剤はポリアクリルアミド、ポリアクリルアミド変性物、硫酸アルミニウム等あり0.5〜3重量%使用される。0.5重量%未満では十分な効果が得られず3重量%を越えても効果の更なる上昇は見られない。
【0009】
本発明にかかる熱膨張性微粒子はスチレン、ポリエチレン、ポリプロピレン、アクリロニトリルと塩化ビニリデンの共重合体、エチレン酢酸ビニル共重合体等の樹脂にプロパン、ブタン、ペンタン、イソブタン等の発泡剤を1種またはそれ以上内包した微粒子である。これらの微粒子の比重は1.0に近いものが均一なスラリーを得るために好ましい。前記熱膨張性樹脂の微粒子には、膨張後の直径が1.0mm〜3.0mm、直径の膨張倍率が3倍以上、かつ膨張開始温度が50〜105℃のものが使用される。膨張後の直径が1.0mm〜3.0mmである理由は1.0mm未満では良好な虫喰模様が形成されず3.0mmを越えると層の組織が粗くなり、強度、硬度が不足する。直径の膨張倍率が3倍以上の理由は鉱物質繊維板の十分な軽量効果得るためである。膨張開始温度が50〜105℃である理由は常温膨張を避けるためと結合剤の硬化開始前に膨張を開始し結合剤の硬化セッティングされる前に膨張は終わるのが好ましいためである。熱膨張性微粒子の使用量は0.5〜7重量%である。0.5重量%より少ないと十分な軽量性が得られず、7重量%を越えると鉱物質繊維板の組織斑、低強度等の問題が生じる。本発明にかかる熱膨張性微粒子は原料スラリーの中に存在するときは微粒であり、比重が1.0近辺であるためスラリー中に容易に均一に分散し製品に密度斑が生じることはない。抄造工程を経てマット状に裁断され乾燥工程において熱膨張性微粒子は加熱され膨張温度に達すると膨張を始めマットはその厚さを増してゆき、配合された結合剤が硬化セッティングされる前に膨張は終わる。マット中の水分が全て蒸発するとほぼドライマットとなり結合剤のセッティングはほぼ終了する。マットの温度は更に上昇してゆくがこの過程で膨張した熱膨張性微粒子は自身の融点に達する。そこで熱膨張性微粒子は溶融破泡し膨張前の容積に戻ってゆき、乾燥終了後結合剤の1部として作用する。膨張した樹脂微粒子により形成された空隙はそのまま残り吸音効果、断熱効果として有効に働く。
【0010】
本発明の鉱物質繊維板は調合工程で鉱物質繊維と有機結合剤と無機質微繊維と凝集剤と熱膨張性微粒子を所定の割合で水に添加し均一に分散し、前記成分の合計量が約5%となるスラリーを得る。スラリーは抄造工程で脱水し、所定寸法に切断した後乾燥硬化して原板が得られる。原板は化粧仕上げ工程に送られ、化粧塗装、あるいは立体切削の後に化粧塗装を施し、最終製品を得る。
従来のピン穴等の吸音加工は素材がポーラスなため不要であり、また全層に亘って虫喰模様状態になっているのでロールによる模様付けも不要である。
【0011】
【実施例】
[実施例1〜4]
表1に示す配合割合で各成分を水に添加し、均一に分散し合計成分が5重量%となるスラリーを得、長網式抄造機により抄造し、乾燥・硬化し、表面切削・化粧切削を施し本発明の鉱物質繊維板を得た。
【0012】
[比較例1〜4]
表1に示す配合割合で各成分を水に添加し、均一に分散し合計成分が5重量%となるスラリーを得、長網式抄造機により抄造し、乾燥・硬化し、表面切削・化粧切削を施し比較用の鉱物質繊維板を得た。
【0013】
実施例1〜4及び比較例1〜4のそれぞれの抄造性及び得られた鉱物質繊維板の物性を測定し表1に示した。
【0014】
【表1】

Figure 0003635806
【0015】
【発明の効果】
表1に示す抄造性及び物性から理解される通り本発明の製造方法によると抄造時濾水時間は20〜23秒と短く、また抄造後厚さを最終製品厚さよりも大巾に薄く設定できるためウエットマットの絶対含水量が大巾に下がるのでライン速度指数も一般従来品を代表する比較例1の100に比べ175〜245と1.7倍以上と極めて生産性に優れる。本発明方法で製造した鉱物質繊維板の物性は乾燥後密度が180〜280kg/m3 と目的の軽量化を達成し、吸音率においても0.60〜0.75と十分な効果が認められる。さらに、その鉱物質繊維板は全層に亘って虫喰模様状態を生じているため、表面切削、立体切削等によって形成した表面に虫喰模様状の自然な凹凸模様が現れ、このため、ロールやサンドブラスト等の機械加工による模様付けが不要となり、自然な凹凸模様を機械加工せずに付与する本発明の大切な目的も十分に達成することができた。[0001]
[Industrial application fields]
TECHNICAL FIELD The present invention relates to a wet manufacturing method of a mineral fiber board that is excellent in lightness, sound absorption, and productivity mainly composed of mineral fibers such as slag and that can give a natural uneven pattern without machining.
[0002]
[Prior art]
Mineral fiberboard by wet manufacturing method, which is mainly made of mineral wool, is used for ceiling interior materials due to its fireproof performance, sound absorption performance and design. However, the conventional mineral fiberboard is required to further improve sound absorption and reduce weight. In addition, conventional design application methods for molded plates by wet manufacturing methods include roll embossing, roll fisher, roll press, sandblast solid processing, etc., all of which require mechanical equipment, so the design application process becomes rate-limiting in productivity. Since the pattern is mechanical, it becomes artificial and regular, and a natural feeling cannot be obtained. Moreover, since the pattern by the roll or sandblast is applied only to the surface layer, the pattern cannot be left in the valley when three-dimensional processing such as a cube is used together. It was practically impossible to leave a pattern over the entire layer of the material by the wet manufacturing method.
[0003]
[Problems to be solved by the invention]
The present invention economically solves the above-mentioned potential problems of mineral fiber board, is excellent in light weight, sound absorption, productivity, and wet production of mineral fiber board that can impart a natural uneven pattern without machining It is to provide a method.
[0004]
[Means for Solving the Problems]
The problems are: mineral fiber 60-90%, organic binder 2-19%, inorganic fine fiber 1-20%, flocculant 0.5-3%, diameter after expansion is 1.0- The composition is composed of 0.5 to 7% by weight of thermally expandable fine particles having a diameter of 3.0 mm, an expansion ratio of a diameter of 3 times or more, and an expansion start temperature of 50 to 105 ° C. The slurry is then cut into a mat through a paper making process, and then in the drying process, the thermally expandable fine particles in the mat are heated and expanded, and the expansion of the thermally expandable fine particles is performed before the setting of the organic binder is set. This is solved by a method for producing a mineral fiberboard, characterized in that after the setting of the organic binder is cured, the thermally expandable fine particles that have expanded are melted and bubble-breaked to form a worm-eating pattern throughout the entire layer. Is done.
[0005]
DETAILED DESCRIPTION OF THE INVENTION
The mineral fiber according to the present invention is mineral cotton, rock wool or the like, and the amount used is 60 to 90% by weight.
[0006]
The organic binder according to the present invention is used in an amount of 2 to 19% by weight for binding components such as mineral fibers in resin, starch, beaten pulp and the like. If the amount is less than 2% by weight, the strength to bind the mineral fiber is insufficient, and there is a problem in maintaining the strength of the mineral fiber board. If the total organic component exceeds 20% by weight, the quasi-incombustibility cannot be cleared in the fire prevention performance. The upper limit of the organic binder is 19% by weight.
[0007]
The inorganic fine fibers according to the present invention are sepiolite, attapulgite, and the like, and contribute to the improvement of strength properties as a binder and a yield improving material for organic binders and thermally expandable resin fine particles. The amount used is 1 to 20% by weight. If it is less than 1% by weight, the effect of improving the yield and improving the physical properties is insufficient, and if it exceeds 20% by weight, the content of the mineral fiber of the main raw material decreases and the density increases, and the paper making process This is not preferable because the production speed decreases due to the deterioration of the drainage.
[0008]
The flocculant according to the present invention includes polyacrylamide, polyacrylamide-modified product, aluminum sulfate and the like, and is used in an amount of 0.5 to 3% by weight. If it is less than 0.5% by weight, a sufficient effect cannot be obtained, and even if it exceeds 3% by weight, no further increase in the effect is observed.
[0009]
The thermally expandable fine particles according to the present invention include one or more blowing agents such as propane, butane, pentane, and isobutane in a resin such as styrene, polyethylene, polypropylene, a copolymer of acrylonitrile and vinylidene chloride, and an ethylene vinyl acetate copolymer. Fine particles encapsulated above. The specific gravity of these fine particles is preferably close to 1.0 in order to obtain a uniform slurry. The fine particles of the heat-expandable resin, the diameter after expansion is 1.0Mm~3.0Mm, more than three times expansion ratio of the diameter, and expansion starting temperature is used those of 50 to 105 ° C.. The reason why the diameter after expansion is 1.0 mm to 3.0 mm is that if the thickness is less than 1.0 mm, a good insect-eating pattern is not formed, and if it exceeds 3.0 mm, the layer structure becomes rough and the strength and hardness are insufficient. The reason why the expansion ratio of the diameter is 3 times or more is to obtain a sufficient light weight effect of the mineral fiber board. The reason why the expansion start temperature is 50 to 105 ° C. is to avoid expansion at room temperature and because it is preferable that the expansion is started before the curing of the binder is started and the expansion is finished before the binder is cured. The amount of the thermally expandable fine particles used is 0.5 to 7% by weight. If the amount is less than 0.5% by weight, sufficient lightness cannot be obtained. The heat-expandable fine particles according to the present invention are fine particles when present in the raw slurry, and since the specific gravity is around 1.0, they are easily and uniformly dispersed in the slurry, and density spots do not occur in the product. After the paper making process, it is cut into a mat shape, and in the drying process, the thermally expandable fine particles are heated and when the temperature reaches the expansion temperature, the mat begins to expand and the mat increases in thickness, expanding before the blended binder is cured and set. Is over. When all the water in the mat is evaporated, the mat becomes almost dry mat and the setting of the binder is almost finished. The temperature of the mat further increases, but the thermally expandable fine particles expanded in this process reach their melting point. Therefore, the thermally expandable fine particles melt and foam and return to the volume before expansion, and act as a part of the binder after drying. The void formed by the expanded resin fine particles remains as it is, and works effectively as a sound absorbing effect and a heat insulating effect.
[0010]
The mineral fiber board of the present invention is a blending process in which mineral fibers, organic binders, inorganic fine fibers, flocculants and thermally expandable fine particles are added to water in a predetermined ratio and uniformly dispersed, and the total amount of the above components is A slurry of about 5% is obtained. The slurry is dehydrated in a paper making process, cut to a predetermined size, and then dried and cured to obtain an original plate. The original plate is sent to the cosmetic finishing process, and after the decorative coating or three-dimensional cutting, the decorative coating is applied to obtain the final product.
Conventional sound absorption processing such as pin holes is unnecessary because the material is porous, and since it is in a worm-eating pattern state over the entire layer, patterning with a roll is also unnecessary.
[0011]
【Example】
[Examples 1 to 4]
Each component is added to water at the blending ratio shown in Table 1 to obtain a slurry which is uniformly dispersed and the total component becomes 5% by weight, made into paper by a long net paper machine, dried and cured, and subjected to surface cutting and cosmetic cutting. To obtain a mineral fiberboard of the present invention.
[0012]
[Comparative Examples 1-4]
Each component is added to water at the blending ratio shown in Table 1 to obtain a slurry which is uniformly dispersed and the total component becomes 5% by weight, made into paper by a long net paper machine, dried and cured, and subjected to surface cutting and cosmetic cutting. To obtain a mineral fiberboard for comparison.
[0013]
The papermaking properties of Examples 1 to 4 and Comparative Examples 1 to 4 and the physical properties of the obtained mineral fiberboard were measured and shown in Table 1.
[0014]
[Table 1]
Figure 0003635806
[0015]
【The invention's effect】
As understood from the papermaking properties and physical properties shown in Table 1, according to the production method of the present invention, the draining time at the time of papermaking is as short as 20 to 23 seconds, and the post-papermaking thickness can be set much thinner than the final product thickness. Therefore, since the absolute water content of the wet mat is greatly reduced, the line speed index is 175 to 245, which is 1.7 times or more higher than that of 100 of Comparative Example 1, which represents a general conventional product, and is extremely excellent in productivity. As for the physical properties of the mineral fiber board produced by the method of the present invention, the density after drying is 180 to 280 kg / m @ 3 and the intended weight reduction is achieved, and a sufficient effect of 0.60 to 0.75 is recognized also in the sound absorption coefficient. Furthermore , since the mineral fiberboard has a worm-eating pattern throughout the entire layer, a natural concavo-convex pattern appears on the surface formed by surface cutting, three-dimensional cutting, etc. The patterning by machining such as sand blasting or the like is no longer necessary, and the important object of the present invention that gives a natural uneven pattern without machining can be sufficiently achieved.

Claims (1)

鉱物質繊維60〜90重量%、有機結合剤2〜19重量%、無機質微繊維1〜20重量%、凝集剤0.5〜3重量%、膨張後の直径が1.0〜3.0mmであり、直径の膨張倍率が3倍以上であり、かつ膨張開始温度が50〜105℃である熱膨張性微粒子0.5〜7重量%を組成成分とし水中に均一に分散してスラリーとし、次に抄造工程を経てマット状に裁断され、続いて乾燥工程において該マット中の熱膨張性微粒子は加熱され膨張し、有機結合剤の硬化セッティングされる前に熱膨張性微粒子の膨張を終わらせ、次いで有機結合剤の硬化セッティング後に膨張した熱膨張性微粒子を溶融破泡させ、全層に亘って虫喰模様状態を生じさせることを特徴とする鉱物質繊維板の製造方法。Mineral fiber 60-90 wt%, organic binder 2-19 wt%, inorganic fine fiber 1-20 wt%, flocculant 0.5-3 wt%, diameter after expansion is 1.0-3.0 mm Yes, the expansion ratio of the diameter is 3 times or more and the expansion start temperature is 50 to 105 ° C., and 0.5 to 7% by weight of thermally expandable fine particles as a composition component is uniformly dispersed in water to form a slurry. In the drying process, the thermally expandable fine particles in the mat are heated and expanded in the drying process, and the expansion of the thermally expandable fine particles is terminated before setting the organic binder to be cured. Next, a method for producing a mineral fiber board, wherein the thermally expandable fine particles expanded after the setting of the organic binder is melted and bubble-breaked to form an insect-eating pattern throughout the entire layer .
JP24100796A 1996-08-26 1996-08-26 Manufacturing method of mineral fiberboard Expired - Lifetime JP3635806B2 (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
JP24100796A JP3635806B2 (en) 1996-08-26 1996-08-26 Manufacturing method of mineral fiberboard
US08/916,360 US5800676A (en) 1996-08-26 1997-08-22 Method for manufacturing a mineral fiber panel
KR1019970040693A KR100245484B1 (en) 1996-08-26 1997-08-25 Method for manufacturing a mineral fiber panel
CNB971176892A CN1148506C (en) 1996-08-26 1997-08-25 Method for mfg. mineral fiber panel

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP24100796A JP3635806B2 (en) 1996-08-26 1996-08-26 Manufacturing method of mineral fiberboard

Publications (2)

Publication Number Publication Date
JPH1072799A JPH1072799A (en) 1998-03-17
JP3635806B2 true JP3635806B2 (en) 2005-04-06

Family

ID=17067949

Family Applications (1)

Application Number Title Priority Date Filing Date
JP24100796A Expired - Lifetime JP3635806B2 (en) 1996-08-26 1996-08-26 Manufacturing method of mineral fiberboard

Country Status (1)

Country Link
JP (1) JP3635806B2 (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4576801B2 (en) * 1999-06-15 2010-11-10 日東紡績株式会社 Radio wave absorbing ceiling panel, method for manufacturing the same, and method for preventing indoor wireless communication failure using the same
JP2006316366A (en) * 2005-05-11 2006-11-24 Jfe Steel Kk Inorganic fiber mat and method for producing the same

Also Published As

Publication number Publication date
JPH1072799A (en) 1998-03-17

Similar Documents

Publication Publication Date Title
US5911818A (en) Acoustical tile composition
KR100245484B1 (en) Method for manufacturing a mineral fiber panel
US1769519A (en) Acoustical material and method of manufacturing same
KR950008561B1 (en) Lightweight building material board
US5071511A (en) Acoustical mineral fiberboard
US5188889A (en) Inorganic board and method of manufacture thereof
US4911788A (en) Method of wet-forming mineral fiberboard with formation of fiber nodules
CA2709690C (en) Acoustic ceiling tiles made with paper processing waste
JP2003140661A (en) Thermoformable acoustic panel
EP3353132B1 (en) Acoustical ceiling tile
EP0347810B1 (en) Acoustical mineral fiberboard and method of manufacturing same
CN103270229A (en) Ceiling tile base mat
JP3635806B2 (en) Manufacturing method of mineral fiberboard
JP2020530588A (en) High noise reduction factor, low density acoustic tile
US3963847A (en) Surface texture for fibrous boards
JP3546607B2 (en) Method of manufacturing mineral fiberboard
JP3843506B2 (en) Manufacturing method of mineral fiberboard
JP4939144B2 (en) Mineral fiberboard and manufacturing method thereof
JPH10502980A (en) Method of manufacturing interior plate board for building
US1491112A (en) Composite board and process for making the same
JP2678781B2 (en) Manufacturing method of lightweight foam mineral wool panel
CA2013566C (en) Method for manufacturing a mineral wool panel
JP4008169B2 (en) Manufacturing method of inorganic board
JPS5887353A (en) Production of moldable nonwoven fabric
US3573083A (en) Surface-layered felted fiber substrate and method of producing same

Legal Events

Date Code Title Description
A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20040309

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20040323

A521 Written amendment

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20040518

A02 Decision of refusal

Free format text: JAPANESE INTERMEDIATE CODE: A02

Effective date: 20040615

A521 Written amendment

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20040811

A911 Transfer of reconsideration by examiner before appeal (zenchi)

Free format text: JAPANESE INTERMEDIATE CODE: A911

Effective date: 20040930

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20041109

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: 20041214

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20041227

R150 Certificate of patent or registration of utility model

Free format text: JAPANESE INTERMEDIATE CODE: R150

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

Free format text: PAYMENT UNTIL: 20090114

Year of fee payment: 4

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

Free format text: PAYMENT UNTIL: 20090114

Year of fee payment: 4

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

Free format text: PAYMENT UNTIL: 20100114

Year of fee payment: 5

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

Free format text: PAYMENT UNTIL: 20110114

Year of fee payment: 6

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

Free format text: PAYMENT UNTIL: 20110114

Year of fee payment: 6

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

Free format text: PAYMENT UNTIL: 20110114

Year of fee payment: 6

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

Free format text: PAYMENT UNTIL: 20120114

Year of fee payment: 7

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

Free format text: PAYMENT UNTIL: 20120114

Year of fee payment: 7

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

Free format text: PAYMENT UNTIL: 20130114

Year of fee payment: 8

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

Free format text: PAYMENT UNTIL: 20130114

Year of fee payment: 8

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

Free format text: PAYMENT UNTIL: 20140114

Year of fee payment: 9

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

EXPY Cancellation because of completion of term