JP4716059B2 - Method for producing higher fatty acid zinc block molded body - Google Patents
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Description
本発明は、静電複写機等の事務機やその他の精密機器等に滑剤、研磨剤、クリーニング助剤、現像助剤などとして用いられる高級脂肪酸亜鉛ブロック成形体の製造方法に関するものである。 The present invention relates to a method for producing a higher fatty acid zinc block molded article used as a lubricant, an abrasive, a cleaning aid, a development aid and the like in office machines such as electrostatic copying machines and other precision equipment.
従来、静電複写機等の事務機に、滑剤、研磨剤、クリーニング助剤、現像助剤などとして高級脂肪酸金属塩が用いられている。この高級脂肪酸金属塩は、最終的には粉状で使用されるが、供給方式として、予め高級脂肪酸金属塩をブロック化して、これをブラシ等で削り取り、必要箇所に供給する方式が実用化されている。 Conventionally, higher fatty acid metal salts have been used in office machines such as electrostatic copying machines as lubricants, abrasives, cleaning aids, development aids, and the like. This higher fatty acid metal salt is finally used in powder form, but as a supply method, a method of blocking the higher fatty acid metal salt in advance, scraping it with a brush, etc., and supplying it to the necessary place has been put to practical use. ing.
上記の応用分野に関連する公知技術として、特開昭57−97572号公報(特許文献1)「電子写真複写機におけるクリーニング方法」があり、助剤組成物としては、特開昭57−73774号公報(特許文献2)「電子写真複写機用クリーニング助剤」がある。また、高級脂肪酸塩の製造方法としては、特許第2796486号公報(特許文献3)記載の溶融固化法、特許第3192371号公報(特許文献4)「金属石鹸ブロック成形用の圧入成形装置及び金属石鹸ブロック成形方法」、特許第3192391号公報(特許文献5)「金属石鹸ブロック成形用の圧入成形ライン及び金属石鹸ブロック成形方法」がある。 As a known technique related to the above application field, there is JP-A-57-97572 (Patent Document 1) “Cleaning method in electrophotographic copying machine”, and an auxiliary composition is disclosed in JP-A-57-73774. There is a gazette (Patent Document 2) “Cleaning aid for electrophotographic copying machine”. Moreover, as a manufacturing method of a higher fatty acid salt, the melt-solidification method described in Japanese Patent No. 2796486 (Patent Document 3), Japanese Patent No. 3192371 (Patent Document 4) “Press-fit molding apparatus and metal soap for metal soap block molding” "Block forming method", Japanese Patent No. 3192391 (Patent Document 5) "Press-fit forming line for metal soap block forming and metal soap block forming method".
しかしながら、いずれも原料物質の脂肪酸金属塩の性状については言及されておらず、得られた高級脂肪酸金属塩ブロック成形体にヒビ、欠け、突起、空隙等が認められ、成形体としての性能が十分得られない場合があった。特に、空隙が発生すると、使用中の削れにバラツキが発生し、品質が安定しない等の問題が発生する場合があった。そのため、ヒビ、欠け、突起、空隙等がなく、品質の安定した高級脂肪酸金属塩ブロック成形体の開発が求められていた。 However, none of the properties of the fatty acid metal salt of the raw material is mentioned, and cracks, chips, protrusions, voids, etc. are recognized in the obtained higher fatty acid metal salt block molded body, and the performance as a molded body is sufficient. In some cases, it could not be obtained. In particular, when voids are generated, there are cases in which there are variations in shaving during use, and the quality is not stable. Therefore, there has been a demand for the development of a higher fatty acid metal salt block molded body having no cracks, chips, protrusions, voids and the like and having stable quality.
本発明は、上記事情に鑑みなされたもので、静電複写機などの事務機に良好に使用できる高級脂肪酸亜鉛ブロック成形体であり、高い耐久性と高度な平滑性を有する高級脂肪酸亜鉛ブロック成形体の製造方法を提供することを目的とするものである。 The present invention has been made in view of the above circumstances, and is a higher fatty acid zinc block molded article that can be used favorably in office machines such as electrostatic copying machines, and has higher durability and higher smoothness. It aims at providing the manufacturing method of a body .
本発明者は、従来の高級脂肪酸金属塩において、前記した問題が起きる理由は、原料の高級脂肪酸金属塩の純度に着目しなかったことにあると考え、上記目的を達成するために鋭意検討を重ねた結果、
(1)高級脂肪酸亜鉛、又は
(2)高級脂肪酸亜鉛:100質量部、及び周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属から選ばれる金属と、低級脂肪酸、高級脂肪酸及び無機炭酸から選ばれる酸との金属塩の少なくとも1種:金属が0質量部を超えて0.10質量部以下となる量を含有してなる組成物
であって、(1)の高級脂肪酸亜鉛又は(2)の組成物中、周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属を総量で0.12質量%以下の濃度(即ち、0質量%を超えて0.12質量%以下)で含有するものを原料とし、これを加熱溶融し、金型に加熱溶融した原料を流し込むなどの方法により冷却固化させて成形体を得るという溶融固化法を用いて得た高級脂肪酸亜鉛ブロック成形体が、高い耐久性と高度な平滑性を有する上述した従来の問題点を解決したものとなることを見出し、本発明をなすに至った。
The present inventor considers that the reason why the above-described problems occur in the conventional higher fatty acid metal salt is that he / she has not paid attention to the purity of the higher fatty acid metal salt as a raw material. As a result,
(1) Higher fatty acid zinc, or (2) Higher fatty acid zinc: 100 parts by mass, a metal selected from Group I alkali metals and Group II alkaline earth metals of the periodic table, lower fatty acids, and higher fatty acids And at least one metal salt with an acid selected from inorganic carbonic acid: a composition comprising a metal in an amount of more than 0 parts by mass and not more than 0.10 parts by mass, the higher fatty acid of (1) In the composition of zinc or (2), the total amount of the Group I alkali metal and the Group II alkaline earth metal in the periodic table is 0.12% by mass or less (that is, 0% by mass exceeding 0% by mass). Obtained by using a melting and solidifying method in which a raw material is used as a raw material, which is heated and melted and cooled and solidified by pouring the heated and melted raw material into a mold to obtain a molded body. Higher fatty acid zinc block moldings are expensive Found that a one has solved the conventional problems described above having durability and high smoothness, the present invention has been accomplished.
従って、本発明は、下記高級脂肪酸亜鉛ブロック成形体の製造方法を提供する。
〔1〕 (A)周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属を総量で0.01質量%以上0.12質量%以下含有する炭素数が8〜20の高級脂肪酸亜鉛を加熱溶融し、これを該高級脂肪酸亜鉛の融点以上に予熱された型内に溶融状態で注入し、これを冷却固化することを特徴とする高級脂肪酸亜鉛ブロック成形体の製造方法。
〔2〕 (A)周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属の総量が0.12質量%以下である炭素数8〜20の高級脂肪酸亜鉛:100質量部に、
(B)周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属から選ばれる金属と、炭素数が7以下の低級脂肪酸、炭素数が8〜20の高級脂肪酸、及び無機炭酸から選ばれる酸との塩の少なくとも1種:金属が0質量部を超えて0.10質量部以下となる量
を混合してなり、かつ(A)成分及び(B)成分中に、周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属を総量で0.01質量%以上0.12質量%以下含有する組成物を加熱溶融し、これを該組成物の融点以上に予熱された型内に溶融状態で注入し、これを冷却固化することを特徴とする高級脂肪酸亜鉛ブロック成形体の製造方法。
〔3〕 (A)ナトリウム、カリウム、マグネシウム及びカルシウムを総量で0.01質量%以上0.12質量%以下含有する炭素数が8〜20の高級脂肪酸亜鉛を加熱溶融し、これを該高級脂肪酸亜鉛の融点以上に予熱された型内に溶融状態で注入し、これを冷却固化することを特徴とする高級脂肪酸亜鉛ブロック成形体の製造方法。
〔4〕 (A)ナトリウム、カリウム、マグネシウム及びカルシウムの総量が0.12質量%以下である炭素数8〜20の高級脂肪酸亜鉛:100質量部に、
(B)ナトリウム、カリウム、マグネシウム及びカルシウムから選ばれる金属と、炭素数が7以下の低級脂肪酸、炭素数が8〜20の高級脂肪酸、及び無機炭酸から選ばれる酸との塩の少なくとも1種:金属が0質量部を超えて0.10質量部以下となる量
を混合してなり、かつ(A)成分及び(B)成分中に、ナトリウム、カリウム、マグネシウム及びカルシウムを総量で0.01質量%以上0.12質量%以下含有する組成物を加熱溶融し、これを該組成物の融点以上に予熱された型内に溶融状態で注入し、これを冷却固化することを特徴とする高級脂肪酸亜鉛ブロック成形体の製造方法。
Therefore, this invention provides the manufacturing method of the following higher fatty acid zinc block molded object.
[1] (A) the periodic table Group I alkali metals and periodic table group II carbon number you containing more than 0.01 wt% 0.12 wt% or less of an alkaline earth metal in a total amount of 8 to 20 A method for producing a higher fatty acid zinc block molded article, comprising heating and melting higher fatty acid zinc, injecting it in a molten state into a mold preheated to a melting point or higher of the higher fatty acid zinc, and cooling and solidifying it.
[2] (A) Higher fatty acid zinc having 8 to 20 carbon atoms in which the total amount of Group I alkali metal and Group II alkaline earth metal of the periodic table is 0.12% by mass or less: 100 parts by mass ,
(B) a metal selected from Group I alkali metals and Group II alkaline earth metals of the periodic table, lower fatty acids having 7 or less carbon atoms, higher fatty acids having 8 to 20 carbon atoms, and inorganic carbonic acid At least one salt with an acid selected from: a metal is mixed in an amount of more than 0 parts by mass and 0.10 parts by mass or less, and the component (A) and the component (B) have a periodic rule Table group I alkali metal and periodic Table group II alkaline earth metal you containing 0.12 wt% 0.01 wt% in total composition heated to melt, which above the melting point of the composition A method for producing a higher fatty acid zinc block molded product, characterized in that it is poured in a molten state into a preheated mold and cooled and solidified.
[3] (A) A higher fatty acid zinc having 8 to 20 carbon atoms containing sodium, potassium, magnesium, and calcium in a total amount of 0.01% by mass to 0.12% by mass is heated and melted, and the higher fatty acid is melted. A method for producing a higher fatty acid zinc block molded article, which comprises pouring in a molten state into a mold preheated to a melting point of zinc or higher and cooling and solidifying the mold.
[4] (A) High fatty acid zinc having 8 to 20 carbon atoms in which the total amount of sodium, potassium, magnesium and calcium is 0.12% by mass or less:
(B) At least one salt of a metal selected from sodium, potassium, magnesium and calcium, a lower fatty acid having 7 or less carbon atoms, a higher fatty acid having 8 to 20 carbon atoms, and an acid selected from inorganic carbonic acid: The amount of metal exceeding 0 parts by mass and 0.10 parts by mass or less
And a composition containing 0.01% by mass or more and 0.12% by mass or less of sodium, potassium, magnesium and calcium in the component (A) and the component (B) by heating and melting, A method for producing a higher fatty acid zinc block molded article, which comprises injecting this in a molten state into a mold preheated to a temperature higher than the melting point of the composition and cooling and solidifying it.
本発明の高級脂肪酸亜鉛ブロック成形体は、従来の高級脂肪酸亜鉛ブロック成形体より高い耐久性と高度な平滑性を有する高級脂肪酸亜鉛ブロック成形体であり、静電複写機などの事務機の滑剤、研磨剤、クリーニング助剤、現像助剤などとして好適に用いることができる。 The higher fatty acid zinc block molded article of the present invention is a higher fatty acid zinc block molded article having higher durability and higher smoothness than conventional higher fatty acid zinc block molded articles, and a lubricant for office machines such as electrostatic copying machines, It can be suitably used as an abrasive, a cleaning aid, a development aid and the like.
本発明の第1の態様の高級脂肪酸亜鉛ブロック成形体は、(A)周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属の総量が0質量%を超えて0.12質量%以下である高級脂肪酸亜鉛の加熱溶融物を冷却固化させることによって得られたものである。また、本発明の第2の態様の高級脂肪酸亜鉛ブロック成形体は、(A)周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属の総量が0質量%を超えて0.12質量%以下である高級脂肪酸亜鉛:100質量部、(B)周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属から選ばれる金属と、低級脂肪酸、高級脂肪酸及び無機炭酸から選ばれる酸との金属塩の少なくとも1種:金属が0質量部を超えて0.10質量部以下となる量を含有してなり、かつ(A)成分及び(B)成分中の、周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属の総量が0質量%を超えて0.12質量%以下である組成物の加熱溶融物を冷却固化させることによって得られたものである。いずれの高級脂肪酸亜鉛ブロック成形体の場合も周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属を総量で0.12質量%以下の濃度(即ち、0質量%を超えて0.12質量%以下)で含有する。なお、本発明の高級脂肪酸亜鉛ブロック成形体の嵩比重は、通常1.090〜1.110である。 In the higher fatty acid zinc block molded article of the first aspect of the present invention, the total amount of (A) group I alkali metal and group II alkaline earth metal of the periodic table exceeds 0% by mass and is 0.12%. It is obtained by cooling and solidifying a heated melt of higher fatty acid zinc having a mass% or less. Further, in the higher fatty acid zinc block molded article of the second aspect of the present invention, the total amount of (A) Periodic Table Group I alkali metal and Periodic Table Group II alkaline earth metal exceeds 0% by mass and is 0. Higher fatty acid zinc of not more than 12% by mass: 100 parts by mass, (B) metal selected from Group I alkali metals and Group II alkaline earth metals of the periodic table, lower fatty acids, higher fatty acids and inorganic At least one metal salt with an acid selected from carbonic acid: the metal is contained in an amount of more than 0 parts by mass and 0.10 parts by mass or less, and in the component (A) and the component (B), It is obtained by cooling and solidifying a heated melt of a composition in which the total amount of Group I alkali metal and Group II alkaline earth metal of the periodic table is more than 0% by mass and 0.12% by mass or less. It is a thing. In the case of any higher fatty acid zinc block molded body, the concentration of the group I alkali metal and group II alkaline earth metal of the periodic table is 0.12% by mass or less in total (ie, exceeding 0% by mass). 0.12% by mass or less). In addition, the bulk specific gravity of the higher fatty acid zinc block molded product of the present invention is usually 1.090 to 1.110.
本発明において、高級脂肪酸亜鉛ブロック成形体は、周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属から選ばれる1種以上、好ましくはナトリウム、カリウム、マグネシウム及びカルシウムから選ばれる1種以上の金属の総量が0.12質量%以下、特に0.10質量%以下であり、好ましくは0.0025質量%以上、より好ましくは0.005質量%以上、特に好ましくは0.01質量%以上である高級脂肪酸亜鉛を原料として使用する。第1の態様の場合は、周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属の総量が0質量%を超えるものを用いる。一方、第2の態様の場合は、周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属を含まないもの(即ち、0質量%)であってもよい。 In the present invention, the higher fatty acid zinc block molded product is at least one selected from Group I alkali metals and Group II alkaline earth metals of the periodic table, preferably sodium, potassium, magnesium and calcium. The total amount of the one or more metals is 0.12% by mass or less, particularly 0.10% by mass or less, preferably 0.0025% by mass or more, more preferably 0.005% by mass or more, particularly preferably 0.01. Higher fatty acid zinc which is at least mass% is used as a raw material. In the case of the first embodiment, the one in which the total amount of Group I alkali metal and Group II alkaline earth metal of the periodic table exceeds 0% by mass is used. On the other hand, in the case of the second aspect, it may be one that does not contain a periodic table group I alkali metal and a periodic table group II alkaline earth metal (that is, 0 mass%).
そして、(A)成分の高級脂肪酸亜鉛、又は(A)成分の高級脂肪酸亜鉛と(B)成分の周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属から選ばれる金属、好ましくはナトリウム、カリウム、マグネシウム及びカルシウムから選ばれる1種以上の金属と、低級脂肪酸、高級脂肪酸及び無機炭酸から選ばれる酸との金属塩の少なくとも1種とを各々所定量含む組成物を加熱溶融し、金型に加熱溶融した原料を流し込むなどの方法により、例えば金型の一端から他端へ順次冷却することにより、冷却固化させて成形体を得る溶融固化法用いて得ることができる。 And (A) higher fatty acid zinc, or (A) higher fatty acid zinc and (B) component periodic table group I alkali metal and periodic table group II alkaline earth metal, Preferably, a composition containing a predetermined amount of at least one metal selected from sodium, potassium, magnesium and calcium and at least one metal salt selected from lower fatty acids, higher fatty acids and inorganic carbonic acid is heated and melted. Then, it can be obtained by a method such as pouring a raw material heated and melted into a mold, for example, by sequentially cooling from one end of the mold to the other end, thereby cooling and solidifying to obtain a molded body.
原料中の周期律表第I族(第1A族)アルカリ金属及び周期律表第II族(第2A族)アルカリ土類金属の含有量を所定量とする理由は、原料中にアルカリ金属及びアルカリ土類金属が特定量を超えて含まれると、得られた高級脂肪酸亜鉛ブロック成形体の耐摩耗性が低下するだけでなく、ヒビ、割れ、突起等が発生しやすくなるためである。即ち、原料中のアルカリ金属及びアルカリ土類金属が特定量を超えて含まれると、製品使用中の安定化が問題となるため、アルカリ金属及びアルカリ土類金属の含有量をその総量で0.12質量%以下、好ましくは0.10質量%以下とする必要がある。 The reason for setting the content of Group I (Group 1A) alkali metal and Periodic Table Group II (Group 2A) alkaline earth metal in the raw material to a predetermined amount is that the alkali metal and alkali in the raw material This is because if the earth metal is contained in excess of a specific amount, not only the wear resistance of the resulting higher fatty acid zinc block molded product is lowered, but cracks, cracks, protrusions and the like are liable to occur. That is, if the alkali metal and alkaline earth metal in the raw material exceeds a specific amount, stabilization during use of the product becomes a problem, so the total content of alkali metal and alkaline earth metal is 0. It is necessary to be 12% by mass or less, preferably 0.10% by mass or less.
また、使用中の削れのバラツキをなくし、安定した品質の高級脂肪酸亜鉛ブロック成形体を得るためには、原料にアルカリ金属又はアルカリ土類金属が含まれていることが必要であるが、原料中のアルカリ金属及びアルカリ土類金属の含有量は、0.0025質量%以上、特に0.005質量%以上、とりわけ0.01質量%以上であることが好ましい。少なすぎると、成形体にヒビ、欠け、突起等が発生する場合がある。 Further, in order to eliminate shaving variations during use and to obtain a high-quality fatty acid zinc block molded product of stable quality, it is necessary that the raw material contains an alkali metal or an alkaline earth metal. The content of alkali metal and alkaline earth metal is preferably 0.0025% by mass or more, more preferably 0.005% by mass or more, and particularly preferably 0.01% by mass or more. If the amount is too small, cracks, chips, protrusions and the like may occur in the molded body.
なお、原料中の高級脂肪酸亜鉛としては特に限定されないが、高級脂肪酸亜鉛を構成する高級脂肪酸の炭素数は8〜20、更には12〜18が好ましく、ミリスチン酸亜鉛、ステアリン酸亜鉛、パルミチン酸亜鉛等が好適に用いられる。また、高級脂肪酸亜鉛としては、粒状又は顆粒状にしたものを使用することができる。 The higher fatty acid zinc in the raw material is not particularly limited, but the higher fatty acid constituting the higher fatty acid zinc preferably has 8 to 20, more preferably 12 to 18, carbon myristate, zinc stearate, zinc palmitate. Etc. are preferably used. Moreover, as higher fatty acid zinc, what was granulated or granulated can be used.
また、第2の態様では、(A)成分の高級脂肪酸亜鉛と、(B)周期律表第I族(第1A族)アルカリ金属及び周期律表第II族(第2A族)アルカリ土類金属から選ばれる金属と、低級脂肪酸、高級脂肪酸及び無機炭酸から選ばれる酸との金属塩の少なくとも1種とを含有し、(A)成分100質量部に対し、(B)成分を、金属が0質量部を超えて、好ましくは0.001質量部以上で、0.10質量部以下となる量で配合した組成物を用いる。この場合も、組成物全体において、周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属の濃度が、これら金属の総量で0.12質量%以下、特に0.10質量%以下であることが好ましく、また、0.0025質量%以上、特に0.005質量%以上、とりわけ0.01質量%以上であることが好ましい。 Further, in the second aspect, the higher fatty acid zinc as the component (A), (B) Group I (Group 1A) alkali metal of the periodic table and Group II (Group 2A) alkaline earth metal of the periodic table And at least one metal salt of an acid selected from lower fatty acids, higher fatty acids, and inorganic carbonic acid, and (A) component is 100 parts by weight with respect to (B) component and the metal is 0 A composition blended in an amount exceeding 0.001 part by mass and preferably 0.10 part by mass or less is used. In this case as well, the concentration of the Group I alkali metal and the Group II alkaline earth metal in the periodic table is 0.12% by mass or less, particularly 0.10% by mass in terms of the total amount of these metals. The content is preferably 0.0025% by mass or more, more preferably 0.005% by mass or more, and particularly preferably 0.01% by mass or more.
(B)成分の金属塩は、その構成金属がアルカリ金属又はアルカリ土類金属であるが、(A)成分の高級脂肪酸亜鉛に含まれるアルカリ金属又はアルカリ土類金属とは作用が異なり、(B)成分の金属塩を併用することにより、得られる高級脂肪酸亜鉛ブロック成形体の衝撃性を、より良好なものとすることができる。この金属としては、例えばリチウム、ナトリウム、カリウム等のアルカリ金属塩、カルシウム、バリウム等のアルカリ土類金属塩が挙げられる。 The component (B) component metal salt is an alkali metal or alkaline earth metal, but the action is different from the alkali metal or alkaline earth metal contained in the higher fatty acid zinc (A) component (B ) By using the metal salt of the component in combination, the impact property of the resulting higher fatty acid zinc block molded product can be made better. Examples of the metal include alkali metal salts such as lithium, sodium and potassium, and alkaline earth metal salts such as calcium and barium.
低級脂肪酸の金属塩としては、特に限定されないが、炭素数が7以下、特に1〜3の脂肪酸の金属塩が好ましく、酢酸ナトリウム、プロピオン酸ナトリウムが好適に用いられる。また、高級脂肪酸の金属塩としては、特に限定されないが、炭素数が8〜30、特に10〜20、とりわけ12〜18が好ましく、好適にはステアリン酸ナトリウムが用いられる。更に、無機炭酸塩としては特に限定されないが、炭酸ナトリウム、炭酸水素ナトリウムが好適に用いられる。 The metal salt of the lower fatty acid is not particularly limited, but a metal salt of a fatty acid having 7 or less carbon atoms, particularly 1 to 3 carbon atoms is preferable, and sodium acetate and sodium propionate are preferably used. The metal salt of the higher fatty acid is not particularly limited, but preferably has 8 to 30, more preferably 10 to 20, particularly 12 to 18 carbon atoms, and sodium stearate is preferably used. Furthermore, although it does not specifically limit as inorganic carbonate, Sodium carbonate and sodium hydrogencarbonate are used suitably.
原料である高級脂肪酸亜鉛の調製法としては、例えば以下に示す方法が挙げられる。なお、ここでは例としてステアリン酸亜鉛について述べるがこの限りではない。まず、ステアリン酸(高級脂肪酸)を多量の水中で攪拌しながら、水酸化ナトリウム(水酸化物)1〜2当量を加えてステアリン酸ナトリウムとする。その後、更に、塩化亜鉛(塩化物)を少しずつ合計で1.5〜3当量添加し、ステアリン酸ナトリウムのナトリウムを亜鉛に置換し、ステアリン酸亜鉛を沈殿生成させる。その後、水洗を施す。水洗は、好ましくは10〜30℃程度の温度で、原料/水=1/5〜1/20割合で、10〜60分洗浄することがよい。その他の高級脂肪酸を用いる場合も同様に、高級脂肪酸の種類を変更して適宜製造することができる。 Examples of the method for preparing the higher fatty acid zinc as a raw material include the following methods. In addition, although zinc stearate is described here as an example, this is not restrictive. First, while stirring stearic acid (higher fatty acid) in a large amount of water, 1 to 2 equivalents of sodium hydroxide (hydroxide) is added to obtain sodium stearate. Thereafter, 1.5 to 3 equivalents of zinc chloride (chloride) is further added little by little to replace sodium stearate with zinc, thereby precipitating zinc stearate. Then, it is washed with water. The washing with water is preferably carried out at a temperature of about 10 to 30 ° C. at a ratio of raw material / water = 1/5 to 1/20 for 10 to 60 minutes. Similarly, when other higher fatty acids are used, they can be appropriately produced by changing the type of higher fatty acids.
次に、高級脂肪酸亜鉛ブロック成形体の製造方法を示す。本発明で使用する型は、使用時に高温になること、熱伝導性や強度が要求されることなどから、金属製の型(以後、単に金型と記す)を用いるとよい。金型の材質は加工性および熱伝導性が良く、取り扱いやすく、高級脂肪酸亜鉛に対して不活性で表面付着の少ないものが好ましく、Al製などのものを用いることが好ましい。 Next, the manufacturing method of a higher fatty acid zinc block molded object is shown. As the mold used in the present invention, a metal mold (hereinafter simply referred to as a mold) is preferably used because it becomes high temperature during use, thermal conductivity and strength are required. The material of the mold is preferably one having good processability and heat conductivity, easy to handle, inert to the higher fatty acid zinc and having less surface adhesion, and preferably made of Al.
高級脂肪酸亜鉛ブロック成形体の形状は、種々あり、それぞれの形状に合った空洞(キャビティ)を備える金型を用いる。例えば、直方体のブロック成形体の製造に金型を用いる場合、金型に製品に対応した寸法の直方体の空洞(キャビティ)を所望個数設けると共に、金型及び/又は金型を載置する台(熱伝導性のよい金属製のものが好ましい)に、ヒーター等の加熱機構及び/又は冷却機構(好ましくは水冷機構)を、必要に応じて成形時に金型に温度勾配をつけられるように設けることができる。金型は、2つ以上に分離する割型が好ましい。 There are various shapes of the higher fatty acid zinc block molded body, and a mold having a cavity (cavity) suitable for each shape is used. For example, when a mold is used to manufacture a rectangular block molded body, a desired number of rectangular parallelepiped cavities (cavities) corresponding to the product are provided in the mold, and a mold and / or a table on which the mold is placed ( Provide a heating mechanism such as a heater and / or a cooling mechanism (preferably a water cooling mechanism) to a metal having good thermal conductivity so that a temperature gradient can be given to the mold during molding as necessary. Can do. The mold is preferably a split mold that is separated into two or more.
製造手順は、例えば以下のとおりとすることができる。まず、金型全体を予め高級脂肪酸亜鉛又は組成物の溶融温度以上に加熱しておき、120〜200℃にて溶融した高級脂肪酸亜鉛又は組成物を金型のキャビティに注ぎ込んで30分〜5時間程度加熱(120〜200℃)を続けた後、金型本体下部又は金型を積置する台に設けられた冷却機構(水冷等)により冷却を行い、これと並行して加熱を金型の下側より順に停止し、高級脂肪酸亜鉛の固化物を下部から徐々に積み上げながら形成する。例えば、まず、下部のヒーター電圧を徐々に下げて温度をゆっくりと低下させ、金型本体下部の温度の低下開始から一定時間後に中央部のヒーター、その後、更に上部のヒーターによる加熱を順次停止する方法を適用することができる。この場合、金型全体の温度が40℃以下になった後、金型を開いて成形体を取り出すことができる。 The manufacturing procedure can be as follows, for example. First, the entire mold is preheated to a temperature higher than the melting temperature of the higher fatty acid zinc or the composition, and the higher fatty acid zinc or the composition melted at 120 to 200 ° C. is poured into the cavity of the mold for 30 minutes to 5 hours. After heating to a certain degree (120 to 200 ° C.), cooling is performed by a cooling mechanism (water cooling or the like) provided on the lower part of the mold body or on a table on which the mold is placed, and in parallel with this, It stops in order from the lower side, and forms a solidified product of higher fatty acid zinc gradually from the bottom. For example, first, the lower heater voltage is gradually lowered to gradually lower the temperature, and after a certain time from the start of lowering of the lower temperature of the mold body, heating by the central heater and then the upper heater are sequentially stopped. The method can be applied. In this case, after the temperature of the entire mold becomes 40 ° C. or less, the mold can be opened and the molded body can be taken out.
以下、実施例及び比較例を示し、本発明を具体的に説明するが、本発明は下記の実施例に制限されるものではない。 EXAMPLES Hereinafter, although an Example and a comparative example are shown and this invention is demonstrated concretely, this invention is not restrict | limited to the following Example.
[実施例1]
ステアリン酸4.5gを30Lの水中で攪拌しながら、水酸化ナトリウムを1.2当量加えてステアリン酸ナトリウムとし、その後、更に、塩化亜鉛を少しずつ合計で1.5当量添加し、ステアリン酸亜鉛を得た。その後、水洗を水温20℃、ステアリン酸亜鉛/水=1/10の割合で、30分行った。得られたステアリン酸亜鉛(ステアリン酸亜鉛Aとする)のアルカリ金属及びアルカリ土類金属の濃度を測定したところ、ナトリウムが0.05質量%であった。
[Example 1]
While stirring 1.2 g of stearic acid in 30 L of water, 1.2 equivalents of sodium hydroxide are added to form sodium stearate, and then 1.5 equivalents of zinc chloride are added little by little, and zinc stearate is added. Got. Thereafter, washing with water was performed for 30 minutes at a water temperature of 20 ° C. and a ratio of zinc stearate / water = 1/10. When the concentration of the alkali metal and alkaline earth metal of the obtained zinc stearate (referred to as zinc stearate A) was measured, sodium was 0.05% by mass.
高級脂肪酸亜鉛中のアルカリ金属及びアルカリ土類金属の濃度は、試料として高級脂肪酸亜鉛1gを蒸留水10mlと濃塩酸3mlを加えて70〜80℃で加温溶解し、その後、放冷・ろ過して、ろ液中のアルカリ金属及びアルカリ土類金属をICP発光分光光度計(IRIS Intrepid II XSP)にて定量することにより測定した。 The concentration of the alkali metal and alkaline earth metal in the higher fatty acid zinc is as follows: 1 g of higher fatty acid zinc as a sample, 10 ml of distilled water and 3 ml of concentrated hydrochloric acid are added and dissolved at 70-80 ° C., and then allowed to cool and filter. Then, the alkali metal and alkaline earth metal in the filtrate were measured by quantifying with an ICP emission spectrophotometer (IRIS Intrepid II XSP).
次に、厚手のアルミニウム板の片面に幅8mm、深さ8mm、長さ400mmの溝が10本設けられた金型10枚と、ヒーターを取り付けたアルミニウム製平板11枚とを両端が平板となるように交互に重ね合わせ、これらをボルトで締めて一体化して固定し、上記溝の長さ方向か上下方向となるように、水冷機構を備える金型載置台に載置した。 Next, 10 dies each having 10 grooves each having a width of 8 mm, a depth of 8 mm, and a length of 400 mm are provided on one side of a thick aluminum plate, and 11 aluminum flat plates to which heaters are attached. In this way, they were alternately superposed, and these were fastened with bolts to be integrated and fixed, and placed on a mold placing table equipped with a water cooling mechanism so as to be in the length direction or vertical direction of the groove.
この金型を160〜200℃に予め予熱し、別途溶融槽で180℃、3時間加熱溶融したステアリン酸亜鉛Aを流し込み、180℃で30分間保持した後、ヒーターへの通電を下部から上部へと順次切り、金型載置台の水冷機構に冷水を循環させた。全体の金型温度が40℃以下になるまで4時間冷却した後、金型を開いてステアリン酸亜鉛のブロック成形体を得た。 This mold is preheated to 160 to 200 ° C in advance, and zinc stearate A heated and melted in a separate melting tank at 180 ° C for 3 hours is poured into it, and maintained at 180 ° C for 30 minutes. Then, cold water was circulated through the water cooling mechanism of the mold mounting table. After cooling for 4 hours until the entire mold temperature reached 40 ° C. or lower, the mold was opened to obtain a block molded body of zinc stearate.
得られたステアリン酸亜鉛ブロック成形体100本について確認したところ、ヒビが1%、欠けが1%発生したが、突起の発生はなかった。また、耐摩耗性を、以下の方法で評価したが、耐摩耗性も良好で、実用に十分耐え得るものであった。表1に結果を示す。 When 100 pieces of the obtained zinc stearate block molded product were confirmed, cracks were generated by 1% and chips were generated by 1%, but no protrusions were generated. Further, the abrasion resistance was evaluated by the following method, but the abrasion resistance was also good and could withstand practical use sufficiently. Table 1 shows the results.
<耐摩耗性>
新東科学社製ヘイドン14DRを使用して測定した。成形体より高さ8mm、幅8mm、長さ10mmのブロックを切り出し、酸化アルミニウム製のやすり(3M社製、品番AL202(50μm))を使用して、荷重100mN(100mm間を5往復、速度17mm/秒)にて8mm×8mm断面を摩耗させた。そのときの摩耗減量を100分率にて表した。このステアリン酸亜鉛ブロック成形体としては0.1〜0.3%が最適範囲である。
<Abrasion resistance>
Measurement was performed using Haydong 14DR manufactured by Shinto Kagaku. A block with a height of 8 mm, a width of 8 mm, and a length of 10 mm is cut out from the molded body, and a load of 100 mN (5 strokes between 100 mm, speed: 17 mm) using an aluminum oxide file (product number AL202 (50 μm) manufactured by 3M). 8 mm × 8 mm cross section was worn at a speed of 1 second / second). The loss on wear at that time was expressed in terms of 100 minutes. The optimal range for this zinc stearate block molding is 0.1 to 0.3%.
[実施例2]
水洗を水温20℃、ステアリン酸亜鉛/水=1/15の割合で、30分行った以外は、実施例1と同様の方法でステアリン酸亜鉛を得た。得られたステアリン酸亜鉛(ステアリン酸亜鉛Bとする)のアルカリ金属及びアルカリ土類金属の濃度を測定したところ、ナトリウムが0.01質量%であった。また、ステアリン酸亜鉛Bを用いて、実施例1と同様の方法でステアリン酸亜鉛ブロック成形体を得、これを評価した。表1に結果を示す。
[Example 2]
Zinc stearate was obtained in the same manner as in Example 1 except that the washing was performed at a water temperature of 20 ° C. and a ratio of zinc stearate / water = 1/15 for 30 minutes. When the alkali metal and alkaline earth metal concentrations of the obtained zinc stearate (referred to as zinc stearate B) were measured, sodium was 0.01% by mass. Moreover, the zinc stearate block molded object was obtained by the method similar to Example 1 using the zinc stearate B, and this was evaluated. Table 1 shows the results.
[実施例3]
水洗を水温20℃、ステアリン酸亜鉛/水=1/10の割合で、15分行った以外は、実施例1と同様の方法でステアリン酸亜鉛を得た。得られたステアリン酸亜鉛(ステアリン酸亜鉛Cとする)のアルカリ金属及びアルカリ土類金属の濃度を測定したところ、ナトリウムが0.10質量%、マグネシウムが0.02質量%であった。また、ステアリン酸亜鉛Bを用いて、実施例1と同様の方法でステアリン酸亜鉛ブロック成形体を得、これを評価した。表1に結果を示す。
[Example 3]
Zinc stearate was obtained in the same manner as in Example 1 except that the washing was performed at a water temperature of 20 ° C. and a ratio of zinc stearate / water = 1/10 for 15 minutes. When the concentration of alkali metal and alkaline earth metal of the obtained zinc stearate (referred to as zinc stearate C) was measured, sodium was 0.10% by mass and magnesium was 0.02% by mass. Moreover, the zinc stearate block molded object was obtained by the method similar to Example 1 using the zinc stearate B, and this was evaluated. Table 1 shows the results.
[実施例4]
実施例2のステアリン酸亜鉛B100質量部にプロピオン酸ナトリウム0.06質量部(ナトリウムとして0.014質量部)混合し、組成物(Na合計0.024質量%)とした。この組成物を用いて、実施例1と同様の方法でステアリン酸亜鉛ブロック成形体を得、これを評価した。表1に結果を示す。
[Example 4]
0.06 parts by mass of sodium propionate (0.014 parts by mass as sodium) was mixed with 100 parts by mass of zinc stearate B of Example 2, to obtain a composition (Na total 0.024% by mass). Using this composition, a zinc stearate block molded body was obtained in the same manner as in Example 1, and this was evaluated. Table 1 shows the results.
[実施例5]
実施例2のステアリン酸亜鉛B100質量部にステアリン酸ナトリウム0.02質量部(ナトリウムとして0.002質量部)混合し、組成物(Na合計0.012質量%)とした。この組成物を用いて、実施例1と同様の方法でステアリン酸亜鉛ブロック成形体を得、これを評価した。表1に結果を示す。
[Example 5]
0.02 parts by mass of sodium stearate (0.002 parts by mass as sodium) was mixed with 100 parts by mass of zinc stearate B of Example 2, to obtain a composition (Na total 0.012% by mass). Using this composition, a zinc stearate block molded body was obtained in the same manner as in Example 1, and this was evaluated. Table 1 shows the results.
[実施例6]
実施例2のステアリン酸亜鉛B100質量部に炭酸水素ナトリウム0.06質量部(ナトリウムとして0.016質量部)混合し、組成物(Na合計0.026質量%)とした。この組成物を用いて、実施例1と同様の方法でステアリン酸亜鉛ブロック成形体を得、これを評価した。表1に結果を示す。
[Example 6]
0.06 parts by mass of sodium hydrogen carbonate (0.016 parts by mass as sodium) was mixed with 100 parts by mass of zinc stearate B of Example 2, to obtain a composition (Na total 0.026% by mass). Using this composition, a zinc stearate block molded body was obtained in the same manner as in Example 1, and this was evaluated. Table 1 shows the results.
[実施例7]
ステアリン酸をパルミチン酸に変更した以外は、実施例1と同様の方法でパルミチン酸亜鉛を得た。その後、実施例1と同様の条件で水洗を実施した。得られたパルミチン酸亜鉛のアルカリ金属及びアルカリ土類金属の濃度を測定したところ、ナトリウムが0.07質量%であった。また、パルミチン酸亜鉛を用いて、実施例1と同様の方法でパルミチン酸亜鉛ブロック成形体を得、これを評価した。表1に結果を示す。
[Example 7]
Zinc palmitate was obtained in the same manner as in Example 1 except that stearic acid was changed to palmitic acid. Thereafter, water washing was performed under the same conditions as in Example 1. When the alkali metal and alkaline earth metal concentrations of the obtained zinc palmitate were measured, sodium was 0.07% by mass. Moreover, the zinc palmitate block molded object was obtained by the method similar to Example 1 using zinc palmitate, and this was evaluated. Table 1 shows the results.
[比較例1]
水洗を水温20℃、ステアリン酸亜鉛/水=1/4の割合で、10分行った以外は、実施例1と同様の方法でステアリン酸亜鉛を得た。得られたステアリン酸亜鉛(ステアリン酸亜鉛Dとする)のアルカリ金属及びアルカリ土類金属の濃度を測定したところ、ナトリウムが0.13質量%であった。また、ステアリン酸亜鉛Dを用いて、実施例1と同様の方法でステアリン酸亜鉛ブロック成形体を得、これを評価した。表1に結果を示す。
[Comparative Example 1]
Zinc stearate was obtained in the same manner as in Example 1 except that the washing was performed at a water temperature of 20 ° C. and a ratio of zinc stearate / water = 1/4 for 10 minutes. The concentration of alkali metal and alkaline earth metal of the obtained zinc stearate (referred to as zinc stearate D) was measured and found to be 0.13% by mass. Moreover, the zinc stearate block molded object was obtained by the method similar to Example 1 using the zinc stearate D, and this was evaluated. Table 1 shows the results.
<ヒビ、欠け、突起合格基準>
ヒビ、突起:発生していないこと
欠け :長さ400mmの製品に対して、長さ5mm未満かつ高さ2mm未満であること
<収率>
ヒビ、欠け、突起発生品を除いた成形体の率を百分率で表示
<Crack, chipping, protrusion acceptance criteria>
Cracks and protrusions: Not occurring Chipping: Less than 5 mm in length and less than 2 mm in height for a product with a length of 400 mm <Yield>
The percentage of the molded product excluding cracks, chips and protrusions is displayed as a percentage.
Claims (4)
(B)周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属から選ばれる金属と、炭素数が7以下の低級脂肪酸、炭素数が8〜20の高級脂肪酸、及び無機炭酸から選ばれる酸との塩の少なくとも1種:金属が0質量部を超えて0.10質量部以下となる量
を混合してなり、かつ(A)成分及び(B)成分中に、周期律表第I族アルカリ金属及び周期律表第II族アルカリ土類金属を総量で0.01質量%以上0.12質量%以下含有する組成物を加熱溶融し、これを該組成物の融点以上に予熱された型内に溶融状態で注入し、これを冷却固化することを特徴とする高級脂肪酸亜鉛ブロック成形体の製造方法。 (A) High fatty acid zinc having 8 to 20 carbon atoms in which the total amount of group I alkali metal and group II alkaline earth metal of the periodic table is 0.12% by mass or less:
(B) a metal selected from Group I alkali metals and Group II alkaline earth metals of the periodic table, lower fatty acids having 7 or less carbon atoms, higher fatty acids having 8 to 20 carbon atoms, and inorganic carbonic acid At least one salt with an acid selected from: a metal is mixed in an amount of more than 0 parts by mass and 0.10 parts by mass or less, and the component (A) and the component (B) have a periodic rule Table group I alkali metal and periodic Table group II alkaline earth metal you containing 0.12 wt% 0.01 wt% in total composition heated to melt, which above the melting point of the composition A method for producing a higher fatty acid zinc block molded product, characterized in that it is poured in a molten state into a preheated mold and cooled and solidified.
(B)ナトリウム、カリウム、マグネシウム及びカルシウムから選ばれる金属と、炭素数が7以下の低級脂肪酸、炭素数が8〜20の高級脂肪酸、及び無機炭酸から選ばれる酸との塩の少なくとも1種:金属が0質量部を超えて0.10質量部以下となる量(B) At least one salt of a metal selected from sodium, potassium, magnesium and calcium, a lower fatty acid having 7 or less carbon atoms, a higher fatty acid having 8 to 20 carbon atoms, and an acid selected from inorganic carbonic acid: The amount of metal exceeding 0 parts by mass and 0.10 parts by mass or less
を混合してなり、かつ(A)成分及び(B)成分中に、ナトリウム、カリウム、マグネシウム及びカルシウムを総量で0.01質量%以上0.12質量%以下含有する組成物を加熱溶融し、これを該組成物の融点以上に予熱された型内に溶融状態で注入し、これを冷却固化することを特徴とする高級脂肪酸亜鉛ブロック成形体の製造方法。And a composition containing 0.01% by mass or more and 0.12% by mass or less of sodium, potassium, magnesium and calcium in the component (A) and the component (B) by heating and melting, A method for producing a higher fatty acid zinc block molded article, which comprises injecting this in a molten state into a mold preheated to a temperature higher than the melting point of the composition and cooling and solidifying it.
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