JP4895010B2 - Higher fatty acid zinc block molded body, method for producing the same, and lubricant for office machine - Google Patents
Higher fatty acid zinc block molded body, method for producing the same, and lubricant for office machine Download PDFInfo
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本発明は、静電複写機等の事務機などにおいて、滑剤、研磨剤、クリーニング助剤、現像助剤等として用いられ、安定かつ好適な特性を有する高級脂肪酸亜鉛ブロック成形体及びその製造方法並びに事務機用滑剤に関する。 The present invention, in an electrostatic copying machine or the like of office equipment, lubricants, abrasives, cleaning aid, used as auxiliary developing agents such as stable and a higher fatty acid zinc block shaped body and a manufacturing method thereof suitable properties and It relates to a lubricant for office machines .
従来より、静電複写機等の事務機において、滑剤、研磨剤、クリーニング助剤あるいは現像助剤として高級脂肪酸金属塩が用いられている。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 as lubricants, abrasives, cleaning aids or development aids in office machines such as electrostatic copying machines. Higher fatty acid metal salts are finally used in powder form, but as a supply method, a method of blocking higher fatty acid metal salts in advance, scraping them with a brush, and supplying them to the necessary places has been put into practical use. Yes.
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「電子写真複写機におけるクリーニング方法」（特許文献１）があり、助剤組成物としては、特開昭５７−７３７７４号公報「電子写真複写機用クリーニング助剤」（特許文献２）がある。また、高級脂肪酸金属塩ブロックの製造方法としては、特許第２７９６４８６号公報「高級脂肪酸金属塩ブロックの製造方法」、特許第３１９２３７１号公報「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「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」（特許文献３〜５）がある。 As a known technique related to the above application field, there is JP-A-57-97572, “Cleaning method in electrophotographic copying machine” (Patent Document 1), and an auxiliary composition is JP-A-57-73774. There is a publication "Cleaning aid for electrophotographic copying machine" (Patent Document 2). Further, as a method for producing a higher fatty acid metal salt block, Japanese Patent No. 2796486, “Method for producing higher fatty acid metal salt block”, Japanese Patent No. 3192371, “Press-fit molding device for metal soap block molding and metal soap block molding method” Patent No. 3192391, “Press-fit line for forming metal soap block and metal soap block forming method” (Patent Documents 3 to 5).
しかしながら、これらの成形装置、成形方法の詳細の中で、原料物質の脂肪酸金属塩の性状については言及されていない。静電複写機等の事務機の滑剤、クリーニング助剤供給として、脂肪酸金属塩のブロックを用いる場合、ブロックの硬さ、ブラシ等による削れ性が一定せず、これまで安定した微量定量フィードが難しいといった問題があった。 However, in the details of these molding apparatuses and molding methods, the properties of the fatty acid metal salt of the raw material are not mentioned. When using fatty acid metal salt blocks to supply lubricants and cleaning aids for office machines such as electrostatic copying machines, the hardness of the blocks and the shaving by brushes are not constant, making stable micro-quantitative feed difficult until now. There was a problem.
本発明は、上記事情に鑑みなされたもので、静電複写機等の事務機などの滑剤、研磨剤、クリーニング助剤、現像助剤等の用途に対して、安定かつ好適な特性を有する高級脂肪酸亜鉛ブロック成形体及びその製造方法並びに事務機用滑剤を提供することを目的とする。 The present invention has been made in view of the above circumstances, and has high and stable characteristics for applications such as lubricants, abrasives, cleaning aids, development aids and the like for office machines such as electrostatic copying machines. It aims at providing the fatty-acid zinc block molded object, its manufacturing method , and the lubricant for office machines .
本発明者らは、上記目的を達成するために鋭意検討を重ねた結果、主成分として高純度の高級脂肪酸亜鉛を用い、これに助剤として特定範囲量の低級脂肪酸、高級脂肪酸あるいは無機炭酸のアルカリ金属塩又はアルカリ土類金属塩を加え、融点以上に加熱溶融した後、予熱された型内に溶融状態で注入し、それを冷却固化させることによって得られた高級脂肪酸亜鉛ブロック成形体が、好適な削れ性と安定した硬さを有し、微量定量フィードが可能になることを見出し、本発明をなすに至った。 The present inventors have made intensive studies in order to achieve the above object, a high-purity of a higher fatty acid zinc as a major component, low-grade fatty acid in a specific range amounts as auxiliaries thereto, high-grade fatty San'a Alternatively, the higher fatty acid zinc obtained by adding an alkali metal salt or alkaline earth metal salt of inorganic carbonate, heating and melting above the melting point, pouring it in a molten state into a preheated mold, and cooling and solidifying it. It has been found that the block molded body has a suitable shaving property and stable hardness, and enables a minute amount of feed to be made, and has led to the present invention.
従って、本発明は、下記に示す高級脂肪酸亜鉛ブロック成形体及びその製造方法並びに事務機用滑剤を提供する。
〔１〕 （Ａ）純度９９．８％以上の高純度高級脂肪酸亜鉛：１００質量部、
（Ｂ）低級脂肪酸、高級脂肪酸、又は無機炭酸のアルカリ金属塩又はアルカリ土類金属塩：金属換算で０．１〜１．０質量部
を含有してな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ことを特徴とする高級脂肪酸亜鉛ブロック成形体。
〔２〕 （Ａ）成分の高級脂肪酸亜鉛が、脂肪酸と亜鉛の金属酸化物又は水酸化物を直接反応させて製造した高級脂肪酸亜鉛であることを特徴とする〔１〕記載の高級脂肪酸亜鉛ブロック成形体。
〔３〕 （Ａ）純度９９．８％以上の高純度高級脂肪酸亜鉛：１００質量部、
（Ｂ）低級脂肪酸、高級脂肪酸、又は無機炭酸のアルカリ金属塩又はアルカリ土類金属塩：金属換算で０．１〜１．０質量部
を含有してなる組成物を加熱溶融し、これを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）成分の高級脂肪酸亜鉛が、脂肪酸と亜鉛の金属酸化物又は水酸化物を直接反応させて製造した高級脂肪酸亜鉛であることを特徴とする〔３〕記載の高級脂肪酸亜鉛ブロック成形体の製造方法。
〔５〕 上記高級脂肪酸亜鉛ブロック成形体からなる事務機用滑剤。
Therefore, this invention provides the higher fatty acid zinc block molded object shown below, its manufacturing method , and the lubricant for office machines .
[1] (A) High purity higher fatty acid zinc having a purity of 99.8% or more: 100 parts by mass,
(B) Low-grade fatty acid, high grade fatty acid, or an alkali metal salt or alkaline earth metal salt of an inorganic carbonate: cooling the molten product in terms of metal in comprising 0.1 to 1.0 parts by weight of the composition A higher fatty acid zinc block molded product obtained by solidifying.
[2] The higher fatty acid zinc block according to [1], wherein the higher fatty acid zinc (A) is a higher fatty acid zinc produced by directly reacting a fatty acid with a metal oxide or hydroxide of zinc. Molded body.
[3] (A) High-purity higher fatty acid zinc having a purity of 99.8% or more: 100 parts by mass,
(B) Low-grade fatty acid, high grade fatty acid, or an alkali metal salt or alkaline earth metal salt of an inorganic carbonate: heating and melting the metal conversion in comprising 0.1 to 1.0 parts by weight of the composition, which Is injected into a mold preheated above the melting point of higher fatty acid zinc in a molten state, and this is cooled and solidified, thereby producing a higher fatty acid zinc block molded body.
[4] The higher fatty acid zinc block according to [3], wherein the higher fatty acid zinc (A) is a higher fatty acid zinc produced by directly reacting a fatty acid with a metal oxide or hydroxide of zinc. Manufacturing method of a molded object.
[5] A lubricant for office machines comprising the higher fatty acid zinc block molded product.
本発明の高級脂肪酸亜鉛ブロック成形体は、クラック発生のトラブルを生ずることなく、硬さのバラツキが小さく、かつブラシ等による削れ量のバラツキの小さいものであり、静電複写機等の事務機やその他の精密機器等における、滑剤、クリーニング助剤等として極めて有効に用いられる。 The higher fatty acid zinc block molded product of the present invention has a small variation in hardness and a small variation in the amount of scraping with a brush or the like without causing troubles of cracks. It is very effectively used as a lubricant and cleaning aid in other precision equipment.
本発明の高級脂肪酸亜鉛ブロック成形体は、
（Ａ）純度９９．８％以上の高純度高級脂肪酸亜鉛、
（Ｂ）低級脂肪酸、高級脂肪酸、又は無機炭酸のアルカリ金属塩又はアルカリ土類金属塩
を含有してなる組成物を加熱溶融し、予熱された型内に溶融状態で注入し、それを冷却固化させてなるものである。
The higher fatty acid zinc block molded article of the present invention,
(A) High purity higher fatty acid zinc having a purity of 99.8% or more,
(B) Low-grade fatty acid, high grade fatty acid, or an alkali metal salt or alkaline earth metal salt of an inorganic carbonate <br/> heating and melting a composition comprising the injection in the molten state in the pre-heated mold It is made by cooling and solidifying it.
本発明の（Ａ）成分である高級脂肪酸亜鉛は、炭素数８〜２０の高級脂肪酸の亜鉛塩であることが好ましく、特に１２〜１８の高級脂肪酸の亜鉛塩であることが好ましい。具体例として、ミリスチン酸亜鉛、パルミチン酸亜鉛、ステアリン酸亜鉛等が挙げられる。 The higher fatty acid zinc as the component (A) of the present invention is preferably a zinc salt of a higher fatty acid having 8 to 20 carbon atoms, particularly preferably a zinc salt of a higher fatty acid having 12 to 18 carbon atoms. Specific examples include zinc myristate, zinc palmitate, zinc stearate and the like.
また、他成分として亜鉛以外の金属塩、例えばＮａ塩、Ｋ塩、Ｃａ塩、Ｍｇ塩が微量含まれていてもよいが、本発明においては、純度９９．８％以上の高純度脂肪酸亜鉛であることが必要である。純度が９９．８％未満であると得られた高級脂肪酸亜鉛ブロック成形体にヒビや割れが発生しやすいばかりでなく、成形体の硬さ、ブラシ等による削れ量が安定せず、バラツキも大きく実用性を損なう。なお、本発明において、純度は原料高級脂肪酸亜鉛を塩酸水にて加熱抽出後、抽出液を回収して純水にて数回洗浄して一定量とする。ＩＣＰ発光分光分析にて定量分析し、各金属量を算出することにより測定することができる。 Further, a metal salt other than zinc, for example, Na salt, K salt, Ca salt, Mg salt, may be contained in a trace amount as other components, but in the present invention, high purity fatty acid zinc having a purity of 99.8% or more is used. It is necessary to be. If the purity is less than 99.8%, the resulting higher fatty acid zinc block molded product is not only susceptible to cracks and cracks, but also the hardness of the molded product, the amount of scraping with a brush, etc. is not stable, and the variation is large. Impairs practicality. In the present invention, the purity of the raw material higher fatty acid zinc is extracted by heating with hydrochloric acid water, and then the extract is recovered and washed several times with pure water to a certain amount. It can be measured by quantitative analysis by ICP emission spectroscopic analysis and calculating the amount of each metal.
高級脂肪酸亜鉛の製法として、一般的には、複分解法（湿式法）と直接法（乾式法）が知られている。複分解法は、高級脂肪酸アルカリ石鹸と亜鉛塩とを水中で反応させ、金属石鹸として高級脂肪酸亜鉛を沈殿させて高級脂肪酸亜鉛を製造する方法である。本方法で造られた高級脂肪酸亜鉛は、反応時に副生する微量のＮａ、Ｋ、Ｃａ等の無機塩を含んでいる。 As a method for producing higher fatty acid zinc, a metathesis method (wet method) and a direct method (dry method) are generally known. The metathesis method is a method for producing a higher fatty acid zinc by reacting a higher fatty acid alkali soap and a zinc salt in water and precipitating the higher fatty acid zinc as a metal soap. The higher fatty acid zinc produced by this method contains a trace amount of inorganic salts such as Na, K, and Ca that are by-produced during the reaction.
一方、直接法は、高級脂肪酸と亜鉛の酸化物又は水酸化物を直接反応させて高級脂肪酸亜鉛を製造する。本製法で造られた高級脂肪酸亜鉛は、反応時に水可溶性の無機塩が副生しないので、通常純度９９．８％以上の生成物が得られる。よって、直接法で得られた高級脂肪酸亜鉛は、本発明の目的を達成するに最適な成分である。この直接法により高級脂肪酸亜鉛を製造する場合、脂肪酸１００質量部に対する亜鉛の酸化物又は水酸化物の配合量は、脂肪酸亜鉛になるような量とすればよいが、好ましくは１０〜５０質量部配合させ、必要によっては加温をして反応させて精製させるものである。 On the other hand, in the direct method, a higher fatty acid zinc is produced by directly reacting a higher fatty acid with an oxide or hydroxide of zinc. Since the higher fatty acid zinc produced by this production method does not produce a water-soluble inorganic salt during the reaction, a product having a purity of 99.8% or more is usually obtained. Therefore, the higher fatty acid zinc obtained by the direct method is an optimal component for achieving the object of the present invention. In the case of producing higher fatty acid zinc by this direct method, the blending amount of zinc oxide or hydroxide with respect to 100 parts by mass of fatty acid may be such an amount that it becomes fatty acid zinc, but preferably 10 to 50 parts by mass. It is made to mix | blend and it is made to refine | purify by making it heat and react as needed.
（Ｂ）成分は本発明の重要な成分であって、低級脂肪酸、高級脂肪酸、又は無機炭酸のアルカリ金属塩又はアルカリ土類金属塩である。低級脂肪酸塩としては、炭素数１〜３、特に１〜２の脂肪酸塩が挙げられ、高級脂肪酸塩としては、炭素数８〜２０、特に１２〜１８の脂肪酸塩が挙げられ、これらの具体例としては、酢酸ナトリウム、酢酸カリウム、酢酸カルシウム、酢酸マグネシウム、蟻酸ナトリウム、蟻酸カリウム、蟻酸カルシウム、蟻酸マグネシウム、ラウリン酸ナトリウム、ラウリン酸カリウム、ラウリン酸マグネシウム、ラウリン酸カルシウム、ステアリン酸ナトリウム、ステアリン酸カリウム、ステアリン酸マグネシウム、ステアリン酸カルシウム、パルミチン酸ナトリウム、パルミチン酸カリウム、パルミチン酸マグネシウム、パルミチン酸カルシウム、ミリスチン酸ナトリウム、ミリスチン酸カリウム、ミリスチン酸マグネシウム、ミリスチン酸カルシウム等が挙げられる。また、無機炭酸塩の具体例としては、炭酸水素カリウム、炭酸水素ナトリウム、炭酸ナトリウム、炭酸カリウム、炭酸カルシウム、炭酸マグネシウム等が挙げられ、特に無機炭酸塩を用いた場合、（Ａ）成分と（Ｂ）成分との反応を更に促進させる触媒作用を与える。これらは１種を単独で、又は２種以上を混合して使用することができる。 Component (B) is an important component of the present invention, a low-grade fatty acid, high-grade fatty acid, or an alkali metal salt or alkaline earth metal salts of inorganic carbonate. Examples of the lower fatty acid salts include fatty acid salts having 1 to 3 carbon atoms, particularly 1 to 2 carbon atoms, and examples of the higher fatty acid salts include fatty acid salts having 8 to 20 carbon atoms, particularly 12 to 18 carbon atoms. As sodium acetate, potassium acetate, calcium acetate, magnesium acetate, sodium formate, potassium formate, calcium formate, magnesium formate, sodium laurate, potassium laurate, magnesium laurate, calcium laurate, sodium stearate, potassium stearate, Magnesium stearate, calcium stearate, sodium palmitate, potassium palmitate, magnesium palmitate, calcium palmitate, sodium myristate, potassium myristate, magnesium myristate, calcium myristate Etc. The. Specific examples of the inorganic carbonate include potassium hydrogen carbonate, sodium hydrogen carbonate, sodium carbonate, potassium carbonate, calcium carbonate, magnesium carbonate and the like, and particularly when an inorganic carbonate is used, the component (A) and ( B) Provides a catalytic action that further accelerates the reaction with the component. These can be used individually by 1 type or in mixture of 2 or more types.
（Ａ）成分と（Ｂ）成分の混合物は、（Ａ）成分の溶融温度以上で加熱溶融されることによって、（Ｂ）成分が（Ａ）成分の反応活性点と反応し、単一の融解ピーク温度を有するものとなる。この加熱溶融物を型に注型し、冷却固化過程で均質に固化させることにより、得られるブロック成形体は、バラツキの少ない硬さを有し、ブラシ等による削れ量が安定した特性を有するものとなる。 The mixture of the component (A) and the component (B) is heated and melted at a temperature equal to or higher than the melting temperature of the component (A), so that the component (B) reacts with the reaction active site of the component (A) and is melted into a single melt It will have a peak temperature. By casting this heated melt into a mold and solidifying it homogeneously in the cooling and solidification process, the resulting block molded body has a hardness with little variation and a characteristic that the amount of scraping by a brush or the like is stable. It becomes.
（Ｂ）成分の添加量は、（Ａ）成分１００質量部に対して当該金属質量換算で０．１〜１．０質量部、好ましくは０．１５〜０．８５質量部である。（Ｂ）成分の添加量が０．１質量部未満では、（Ａ）、（Ｂ）成分を含有する組成物が加熱溶融によって単一ピーク温度を有するものにならず、結果として本発明の目的としている性状のブロック成形体が得られず、１．０質量部より多い量では、冷却固化した高級脂肪酸亜鉛ブロック成形体中に未反応の（Ｂ）成分又はその塩が、ブロック成形体の割れ、欠け等の核となって、実用的強度を有するブロック成形体が得られなかったり、ブラシ等による削れ量のバラツキが大きくなる。 The addition amount of (B) component is 0.1-1.0 mass part in conversion of the said metal mass with respect to 100 mass parts of (A) component, Preferably it is 0.15-0.85 mass part. When the addition amount of component (B) is less than 0.1 parts by mass, the composition containing components (A) and (B) does not have a single peak temperature by heating and melting, and as a result, the object of the present invention If the block molded product having the properties described above is not obtained and the amount is more than 1.0 part by mass, the unreacted component (B) or the salt thereof is cracked in the block molded product in the cooled and solidified higher fatty acid zinc block molded product. As a result, a block molded body having a practical strength cannot be obtained due to the core of chipping or the like, and the variation in the amount of scraping with a brush or the like increases.
次に、高級脂肪酸亜鉛ブロック成形体の製造方法について説明する。本発明の高級脂肪酸亜鉛の棒状のブロック成形体を得る方法として、（Ａ）、（Ｂ）成分からなる組成物を、（Ａ）成分である高級脂肪酸亜鉛の融点以上、通常１４０℃以上、特に１５０〜２００℃に加熱溶融し、（Ａ）成分である高級脂肪酸亜鉛の融点以上、特に１４０〜１６０℃に予熱された金型に注入し、その後金型を冷却し、固化させる。金型温度が４０℃以下、好ましくは１５〜３５℃で脱型すればブロック状の成形体が得られる。この条件を満たせば、本発明は型構造や、冷却条件に規定はなく、特許第２７９６４８６号公報や特許第３１９２３９１号公報等で紹介されている公知のいずれの方法を用いても製造することができる。 Next, the manufacturing method of a higher fatty acid zinc block molded object is demonstrated. As a method of obtaining the higher fatty acid zinc rod-shaped block molded product of the present invention, the composition comprising the components (A) and (B) is a melting point of the higher fatty acid zinc as the component (A), usually 140 ° C. or higher. It is heated and melted at 150 to 200 ° C., and poured into a mold preheated to a melting point of higher fatty acid zinc (A) component, particularly 140 to 160 ° C., and then the mold is cooled and solidified. If the mold is removed at a mold temperature of 40 ° C. or lower, preferably 15 to 35 ° C., a block-shaped molded body is obtained. If this condition is satisfied, the present invention can be manufactured using any of the known methods introduced in Japanese Patent No. 2796486, Japanese Patent No. 3192391, etc. without any restrictions on the mold structure or cooling conditions. it can.
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］
（Ａ）成分としてステアリン酸と水酸化亜鉛を反応させ、ステアリン酸亜鉛以外の金属元素化合物総量が２０ｐｐｍである純度９９．９％以上の直接法で造られた高純度ステアリン酸亜鉛Ａ １，０００ｇ（１００質量部）と、（Ｂ）成分としてステアリン酸ナトリウム（和光純薬製試薬）５０ｇ（Ｎａ金属換算０．３７５質量部）を３Ｌの加熱槽付品川ミキサーに仕込み、１５０〜１６０℃の溶融状態で２時間撹拌熟成した。
成形体を作るのに厚手のアルミニウム板の片面に幅１０ｍｍ、深さ１０ｍｍ、長さ４５０ｍｍの溝が１０本縦に彫られた金型に、ヒーターを内蔵したアルミニウム製平版２枚を両側に組み合わせ、これら３枚をボルトで締めて固定した。その金型を冷却機構を備えたステンレス製の冷却盤上にセットした。
次に、予め１５０〜１６０℃に予熱しておいた金型に先程の溶融熟成した液を注入し、２０分間保持した後、金型のヒーターを切り、冷却盤に冷水を循環させて金型を冷却させた。４時間後、金型温度が３６℃となり、４０℃以下になったことを確認して、金型を開いてステアリン酸亜鉛の成形体を作製した。得られた成形体を用いて、硬さ、削れ量を５本の成形体について評価した。これらの評価結果を成形収率と共に表１に示す。硬さ、削れ量共バラツキの小さい、ステアリン酸亜鉛ブロック成形体を得た。
[Example 1]
(A) High-purity zinc stearate A 1,000 g produced by a direct method having a purity of 99.9% or more in which stearic acid and zinc hydroxide are reacted as components and the total amount of metal element compounds other than zinc stearate is 20 ppm (100 parts by mass) and 50 g of sodium stearate (reagent made by Wako Pure Chemical Industries) as a component (B) (0.375 parts by mass in terms of Na metal) were charged into a 3 L heating tank equipped Shinagawa mixer and melted at 150 to 160 ° C. The mixture was aged with stirring for 2 hours.
To make a molded body, combine two aluminum flat plates with built-in heaters on both sides of a mold with 10 grooves 10mm wide, 10mm deep and 450mm long on one side of a thick aluminum plate. These three pieces were fixed with bolts. The mold was set on a stainless steel cooling plate equipped with a cooling mechanism.
Next, the previously melted and aged solution is poured into a mold preheated to 150 to 160 ° C., held for 20 minutes, the mold heater is turned off, and cold water is circulated through the cooling plate to mold the mold. Was allowed to cool. After 4 hours, it was confirmed that the mold temperature was 36 ° C. and 40 ° C. or less, and the mold was opened to produce a molded body of zinc stearate. Using the obtained molded body, the hardness and the amount of scraping were evaluated for 5 molded bodies. These evaluation results are shown in Table 1 together with the molding yield. A zinc stearate block molded body having small variations in both hardness and chipping amount was obtained.
［実施例２］
（Ａ）成分として実施例１と同様のステアリン酸亜鉛Ａ １，０００ｇ（１００質量部）と、（Ｂ）成分としてステアリン酸マグネシウム（和光純薬製試薬）１００ｇ（Ｍｇ金属換算０．４１０質量部）を３Ｌの加熱槽付品川ミキサーに仕込み、１５０〜１６０℃の溶融状態で２時間撹拌熟成した。溶融熟成した液体を実施例１と同様にしてステアリン酸亜鉛成形体を作製した。得られた成形体を用いて、硬さ、削れ量を５本の成形体について評価した。表１に結果を示す。硬さ、削れ量共バラツキの小さいステアリン酸亜鉛ブロック成形体を得た。
[Example 2]
As the component (A), 1,000 g (100 parts by mass) of zinc stearate A as in Example 1, and as the component (B) 100 g of magnesium stearate (a reagent manufactured by Wako Pure Chemical Industries) (0.410 parts by mass in terms of Mg metal). ) Was placed in a 3 L heating tank equipped Shinagawa mixer, and aged and aged in a molten state at 150 to 160 ° C. for 2 hours. A zinc stearate molded body was produced from the melt-aged liquid in the same manner as in Example 1. Using the obtained molded body, the hardness and the amount of scraping were evaluated for 5 molded bodies. Table 1 shows the results. A zinc stearate block molded product having small variations in hardness and scraping amount was obtained.
［実施例３］
実施例１の（Ｂ）成分のステアリン酸ナトリウムの配合量を８０ｇ（Ｎａ金属換算０．６００質量部）とする以外は、同様な条件でステアリン酸亜鉛成形体を作製した。得られた成形体を用いて、硬さ、削れ量を５本の成形体について評価した。表１に結果を示す。硬さ、削れ量共バラツキの小さい、ステアリン酸亜鉛ブロック成形体を得た。
[Example 3]
A zinc stearate molded body was produced under the same conditions except that the amount of sodium stearate as the component (B) in Example 1 was changed to 80 g (0.600 parts by mass in terms of Na metal). Using the obtained molded body, the hardness and the amount of scraping were evaluated for 5 molded bodies. Table 1 shows the results. A zinc stearate block molded body having small variations in both hardness and chipping amount was obtained.
［実施例４］
実施例１の（Ｂ）成分をＮａＨＣＯ3 １４ｇ（Ｎａ金属換算０．３８５質量部）とする以外は、同様な条件でステアリン酸亜鉛成形体を作製した。得られた成形体を用いて硬さ、削れ量を５本の成形体について評価した。表１に結果を示す。硬さ、削れ量共バラツキの小さいステアリン酸亜鉛ブロック成形体を得た。
[Example 4]
A zinc stearate molded body was produced under the same conditions except that the component (B) of Example 1 was 14 g of NaHCO 3 (0.385 parts by mass in terms of Na metal). Five molded bodies were evaluated for hardness and scraping amount using the obtained molded bodies. Table 1 shows the results. A zinc stearate block molded product having small variations in hardness and scraping amount was obtained.
［実施例５］
実施例１の（Ｂ）成分をＮａＨＣＯ3 ２８ｇ（Ｎａ金属換算０．７６７質量部）とする以外は、同様な条件でステアリン酸亜鉛成形体を作製した。得られた成形体を用いて、硬さ、削れ量を５本の成形体で評価した。表１に結果を示す。硬さ、削れ量共バラツキの小さいステアリン酸亜鉛ブロック成形体を得た。
[Example 5]
A zinc stearate molded body was produced under the same conditions except that the component (B) of Example 1 was 28 g of NaHCO 3 (0.767 parts by mass in terms of Na metal). Using the obtained molded body, the hardness and the amount of scraping were evaluated with 5 molded bodies. Table 1 shows the results. A zinc stearate block molded product having small variations in hardness and scraping amount was obtained.
［実施例６］
実施例１の（Ｂ）成分をＮａ2ＣＯ3 １０ｇ（Ｎａ金属換算０．４３４質量部）とする以外は、同様な条件でステアリン酸亜鉛成形体を作製した。得られた成形体を用いて、硬さ、削れ量を５本の成形体で評価した。表１に結果を示す。硬さ、削れ量共バラツキの小さい、ステアリン酸亜鉛ブロック成形体を得た。
[Example 6]
A zinc stearate molded body was produced under the same conditions except that the component (B) of Example 1 was changed to 10 g of Na 2 CO 3 (0.434 parts by mass in terms of Na metal). Using the obtained molded body, the hardness and the amount of scraping were evaluated with 5 molded bodies. Table 1 shows the results. A zinc stearate block molded body having small variations in both hardness and chipping amount was obtained.
［実施例７］
実施例１の（Ｂ）成分をＣＨ3ＣＯＯＫ １０ｇ（Ｋ金属換算０．３９９質量部）とする以外は、同様な条件でステアリン酸亜鉛成形体を作製した。得られた成形体を用いて、硬さ、削れ量を５本の成形体で評価した。表１に結果を示す。硬さ、削れ量共バラツキの小さい、ステアリン酸亜鉛ブロック成形体を得た。
[Example 7]
A zinc stearate molded body was produced under the same conditions except that the component (B) of Example 1 was CH 3 COOK 10 g (0.399 parts by mass in terms of K metal). Using the obtained molded body, the hardness and the amount of scraping were evaluated with 5 molded bodies. Table 1 shows the results. A zinc stearate block molded body having small variations in both hardness and chipping amount was obtained.
［実施例８］
実施例１中の（Ａ）成分としてステアリン酸亜鉛以外の金属元素化合物総量が３１ｐｐｍである純度９９．９％以上の直接法で造られた高純度ステアリン酸亜鉛Ｂ １，０００ｇ（１００質量部）とする以外は、同様な条件でステアリン酸亜鉛成形体を作製した。得られた成形体を用いて、硬さ、削れ量を５本の成形体で評価した。表１に結果を示す。硬さ、削れ量共バラツキの小さい、ステアリン酸亜鉛ブロック成形体を得た。
[Example 8]
1,000 g (100 parts by mass) of high-purity zinc stearate B produced by a direct method having a purity of 99.9% or more, in which the total amount of metal element compounds other than zinc stearate is 31 ppm as component (A) in Example 1 Except for the above, a zinc stearate molded body was produced under the same conditions. Using the obtained molded body, the hardness and the amount of scraping were evaluated with 5 molded bodies. Table 1 shows the results. A zinc stearate block molded body having small variations in both hardness and chipping amount was obtained.
［比較例１］
（Ａ）成分としてステアリン酸亜鉛以外の金属化合物（Ｎａ、Ｃａ、Ｆｅ、Ｔｉ等）総量が０．３５％含まれている複分解法（湿式法）で製造されたステアリン酸亜鉛Ｃ（堺化学工業（株）製ＳＺ−２０００）１，０００ｇ（１００質量部）のみを３Ｌの加熱槽付品川ミキサーに仕込み、１５０〜１６０℃の溶融状態で２時間撹拌熟成した。溶融物を実施例１と同様な手順でステアリン酸亜鉛成形体を作製した。得られた成形体を用いて、硬さ、削れ量を５本の成形体について評価した。表２に結果を示す。硬さ、削れ量共バラツキが大きく、得られたステアリン酸亜鉛成形体は安定性に欠けるものであった。
[Comparative Example 1]
Zinc stearate C produced by a metathesis method (wet method) containing 0.35% of the total amount of metal compounds (Na, Ca, Fe, Ti, etc.) other than zinc stearate as component (A) Only 1,000 g (100 parts by mass) of SZ-2000 manufactured by Co., Ltd. was charged into a 3 L Shinagawa mixer with a heating tank, and stirred and aged for 2 hours in a molten state at 150 to 160 ° C. A zinc stearate molded body was produced from the melt in the same procedure as in Example 1. Using the obtained molded body, the hardness and the amount of scraping were evaluated for 5 molded bodies. Table 2 shows the results. Both the hardness and the amount of chipping varied greatly, and the obtained zinc stearate molded article lacked stability.
［比較例２］
（Ａ）成分として、実施例１の（Ａ）成分と同じステアリン酸亜鉛Ａ １，０００ｇ（１００質量部）、（Ｂ）成分なしとする以外は、実施例１と同様な手順でステアリン酸亜鉛ブロック成形体を得た。金型から取り出した成形体はいずれも脆く、欠けのあるもので満足な形状を有する成形体は得られなかった。得られた成形体を用いて、硬さ、削れ量を５本の成形体について評価した。表２に結果を示す。硬さは柔らかく、成形体は全てクラックが入り、実用的ブロック成形体を得ることはできなかった。削れ量も多く、またバラツキも大きく、実用的な特性を得ることができなかった。
[Comparative Example 2]
As the component (A), zinc stearate in the same procedure as in Example 1 except that 1,000 g (100 parts by mass) of zinc stearate A same as the component (A) of Example 1 and no component (B) are used. A block molded body was obtained. All of the molded articles taken out from the mold were brittle, and there were no chips with satisfactory shapes. Using the obtained molded body, the hardness and the amount of scraping were evaluated for 5 molded bodies. Table 2 shows the results. The hardness was soft, and all the molded bodies were cracked, and a practical block molded body could not be obtained. The amount of shaving was large and the variation was large, so practical characteristics could not be obtained.
［比較例３］
実施例１の（Ｂ）成分のステアリン酸ナトリウムの配合量を１６０ｇ（Ｎａ金属換算１．２００質量部）とする以外は、実施例１と同様にステアリン酸亜鉛成形体を得た。得られた成形体を用いて、硬さ、削れ量を５本の成形体について評価した。表２に結果を示す。硬さについては形状を維持する実用的な値を得ることができたが、硬さ、削れ量についてはバラツキが大きく、本発明の目的とするバラツキの小さい硬さと、ブラシ等による削れ量の安定したステアリン酸亜鉛ブロック成形体を得ることができなかった。
[Comparative Example 3]
A zinc stearate molded article was obtained in the same manner as in Example 1 except that the blending amount of sodium stearate as the component (B) in Example 1 was 160 g (Na metal equivalent: 1.200 parts by mass). Using the obtained molded body, the hardness and the amount of scraping were evaluated for 5 molded bodies. Table 2 shows the results. As for the hardness, a practical value for maintaining the shape could be obtained. However, the hardness and the amount of scraping varied greatly, and the hardness of the object of the present invention with small variation and the stability of the amount of shaving by a brush or the like. The obtained zinc stearate block molding could not be obtained.
《ステアリン酸亜鉛ブロック成形体の評価方法》
＜硬さ測定＞
ＪＩＳ−Ｚ−２２４４に準拠。マツザワ社製デジタル微小硬度計ＭＭＴ−７型を使用して測定する。一定の太さの針を荷重１ｍＮで成形体に押し当て、その時できる圧痕の対角線の距離を決めることで自動的に硬さが算出される。数字が大きいほど硬いことになるが、本発明の高級脂肪酸亜鉛ブロック成形体では４．５〜５．５の硬さが要求される。
<< Method for evaluating zinc stearate block molded article >>
<Hardness measurement>
Conforms to JIS-Z-2244. It is measured using a digital microhardness meter MMT-7 manufactured by Matsuzawa. The hardness is automatically calculated by pressing a needle with a constant thickness against the molded body with a load of 1 mN and determining the diagonal distance of the indentation that can be made at that time. The higher the number, the harder it is, but the higher fatty acid zinc block molded product of the present invention requires a hardness of 4.5 to 5.5.
＜削れ量測定＞
削れ量測定は、図１に示す評価測定機を用いて行う。まず、上記で得られた１０ｍｍ角のステアリン酸亜鉛ブロック成形体を２５０ｍｍの長さにカットし、この側面に鉄製の背材を両面粘着テープで固定して測定サンプル（ステアリン酸亜鉛バー１）を作製する。次に、研磨材である径１０ｍｍの円筒状ナイロンブラシ２をモーター３に取り付け、更に、両端に荷重調整錘７と試料把持治具５を設けたアーム６の試料把持治具５に、ステアリン酸亜鉛バー１を背材４にて固定し、ステアリン酸亜鉛バー１をブラシ２と接触させる。ブラシ２がモーター３の駆動で回転し、ステアリン酸亜鉛バー１は設定荷重でブラシ２と接触して削られるものである。
本実施例、比較例での削れ量測定の条件は次の通りである。下記条件での削れ量（ｍｇ）を測定する。
試料にかかる荷重：３００ｇ
ブラシの回転速度：３３３ｒｐｍ
試験時間 ：１０分
<Measurement of scraping amount>
The amount of scraping is measured using the evaluation measuring machine shown in FIG. First, the 10 mm square zinc stearate block molded body obtained above was cut into a length of 250 mm, and an iron back material was fixed to this side surface with a double-sided adhesive tape to prepare a measurement sample (zinc stearate bar 1). Make it. Next, a cylindrical nylon brush 2 having a diameter of 10 mm, which is an abrasive, is attached to the motor 3, and stearic acid is applied to the sample gripping jig 5 of the arm 6 provided with the load adjusting weight 7 and the sample gripping jig 5 at both ends. The zinc bar 1 is fixed with the backing material 4, and the zinc stearate bar 1 is brought into contact with the brush 2. The brush 2 is rotated by the drive of the motor 3, and the zinc stearate bar 1 is scraped in contact with the brush 2 with a set load.
The conditions for measuring the amount of wear in this example and the comparative example are as follows. The amount of abrasion (mg) is measured under the following conditions.
Load applied to the sample: 300 g
Brush rotation speed: 333 rpm
Test time: 10 minutes
１ ステアリン酸亜鉛バー
２ ブラシ
３ モーター
５ 試料把持治具
６ アーム
７ 荷重調整錘
1 Zinc stearate bar 2 Brush 3 Motor 5 Sample gripping jig 6 Arm 7 Load adjustment weight
Claims (8)
（Ｂ）低級脂肪酸、高級脂肪酸、又は無機炭酸のアルカリ金属塩又はアルカリ土類金属塩：金属換算で０．１〜１．０質量部
を含有してな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ことを特徴とする高級脂肪酸亜鉛ブロック成形体。 (A) High purity higher fatty acid zinc having a purity of 99.8% or more: 100 parts by mass,
(B) Low-grade fatty acid, high grade fatty acid, or an alkali metal salt or alkaline earth metal salt of an inorganic carbonate: cooling the molten product in terms of metal in comprising 0.1 to 1.0 parts by weight of the composition A higher fatty acid zinc block molded product obtained by solidifying.
（Ｂ）低級脂肪酸、高級脂肪酸、又は無機炭酸のアルカリ金属塩又はアルカリ土類金属塩：金属換算で０．１〜１．０質量部
を含有してなる組成物を加熱溶融し、これを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。 (A) High purity higher fatty acid zinc having a purity of 99.8% or more: 100 parts by mass,
(B) Low-grade fatty acid, high grade fatty acid, or an alkali metal salt or alkaline earth metal salt of an inorganic carbonate: heating and melting the metal conversion in comprising 0.1 to 1.0 parts by weight of the composition, which Is injected into a mold preheated above the melting point of higher fatty acid zinc in a molten state, and this is cooled and solidified, thereby producing a higher fatty acid zinc block molded body.
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