JP4861543B2 - Method for producing ink backflow preventive composition for writing instrument - Google Patents
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本発明は、筆記具用インキ逆流防止体組成物の製造方法に関する。更に詳細には、インキ収容筒内に収容したインキの後端面にインキの消費に従い前進する高粘度流体である筆記具用インキ逆流防止体組成物の製造方法に関する。 The present invention relates to a method for producing an ink backflow preventive composition for a writing instrument. More specifically, the present invention relates to a method for producing an ink backflow preventive composition for a writing instrument, which is a high-viscosity fluid that moves forward in accordance with ink consumption to the rear end surface of ink stored in an ink storage cylinder.
パイプ状のインキ収容管内に充填されたインキを、インキ誘導芯等を介することなく、直接ペン体へ導出させる構造の筆記具として、油性ボールペンが従来から汎用されている。このタイプの油性ボールペンに適用されるインキは数千乃至数万ｍＰａ・ｓの高粘度インキであり、その高い粘性により筆記には高い筆記圧が必要であった。近年、前記油性ボールペンの構造と中粘度（数十〜数百ｍＰａ・ｓ）の水性インキを組み合わせた水性ボールペンが多用されてきている。 An oil-based ballpoint pen has been widely used as a writing instrument having a structure in which ink filled in a pipe-shaped ink storage tube is directly led to a pen body without using an ink guide core or the like. The ink applied to this type of oil-based ballpoint pen is a high-viscosity ink of several thousand to several tens of thousands of mPa · s, and a high writing pressure is required for writing due to its high viscosity. In recent years, water-based ballpoint pens that combine the structure of the oil-based ballpoint pen with a water-based ink having a medium viscosity (several tens to several hundreds mPa · s) have been widely used.
この種の水性インキは油性インキに比較して粘度が低いため、軽い筆記圧で筆記をすることができるが、その粘性の低さによりインキ収容管後端方向へインキが流出しやすいという欠点がある。そのために、通常インキ収容管内のインキ後端面に高粘度流体であるインキ逆流防止体を配することが必須となっている。 Since this type of water-based ink has a lower viscosity than oil-based inks, it can be written with light writing pressure, but due to its low viscosity, the ink tends to flow out toward the rear end of the ink containing tube. is there. For this reason, it is essential to provide an ink backflow prevention body, which is a highly viscous fluid, on the rear end surface of the ink in the normal ink storage tube.
インキ逆流防止体には主に前記したインキ逆流防止性と、インキの消費に従ってインキと共に移動し筆記を円滑にさせるインキ追従性という相反する二つの特性が要求される。インキ逆流防止性を向上させるためにインキ逆流防止体を硬くするとインキ追従性が劣ってしまい、インキ追従性を良好にするためにインキ逆流防止体を軟らかくすれば、容易にインキ逆流が発生してしまう。 The ink backflow prevention body is required to have two contradictory characteristics, namely, the ink backflow prevention performance described above and the ink follow-up performance that moves together with the ink according to the consumption of the ink and smoothes writing. If the ink backflow prevention body is hardened to improve the ink backflow prevention property, the ink followability will be inferior, and if the ink backflow prevention body is made soft to improve the ink followability, ink backflow will easily occur. End up.
従来、これら要求性能を具備するインキ逆流防止体を提供する目的で種々の提案がなされている。例えば特公平６−４７３１８号公報には液状ポリブテンをベースオイルとし、微粒子シリカ、金属セッケン類或いはベントナイト等で増粘させたインキ逆流防止体が、また特開平１１−１６５４８６号公報等にはシリコーンオイルをベースオイルとし、微粒子シリカ、ベンジリデンソルビトール或いはアミノ酸誘導体等で増粘させたインキ逆流防止体が開示されている。 Conventionally, various proposals have been made for the purpose of providing an ink backflow preventer having these required performances. For example, Japanese Patent Publication No. 6-47318 discloses an ink backflow preventer using liquid polybutene as a base oil and thickened with fine particle silica, metal soap, bentonite or the like, and Japanese Patent Application Laid-Open No. 11-165486 discloses a silicone oil. An ink backflow preventer is disclosed in which the base oil is thickened with fine particle silica, benzylidene sorbitol, an amino acid derivative, or the like.
前記従来のインキ逆流防止体のうち前者はベースオイルに用いられている液状ポリブテンがインキ中の成分である染料、界面活性剤、各種添加剤等との親和性が高いため、インキ逆流防止体組成物の一部がインキ中へ移行したり或いはインキ中の一部の成分がインキ逆流防止体中へ移行して、インキ逆流防止体やインキの物性が変化し、インキ逆流防止性能の低下やインキの変質、変色等の問題を発生しがちであった。 Among the conventional ink backflow prevention bodies, the former is a liquid polybutene used in base oil, which has high affinity with dyes, surfactants, various additives, etc., which are components in the ink. Part of the ink moves into the ink, or some of the components in the ink move into the ink backflow prevention body, the ink backflow prevention body and the ink physical properties change, and the ink backflow prevention performance decreases and the ink There was a tendency to cause problems such as alteration and discoloration.
また、後者のシリコーンオイルをベースオイルとしたインキ逆流防止体の場合、剪断力が付加された際に粘度の低下が著しく、剪断力を取り去った後に元の粘度に回復するまでに長時間を要する。更に、該インキ逆流防止体を長期間保管すると徐々にゲル強度が低下し、十分なインキ逆流防止性能が得られなくなり、チップ上向き（正立）状態での放置或いは衝撃によるインキ漏出等の不具合を発生する虞があった。 Further, in the case of the ink backflow preventer using the latter silicone oil as a base oil, the viscosity is remarkably lowered when a shearing force is applied, and it takes a long time to recover the original viscosity after removing the shearing force. Furthermore, when the ink backflow preventive body is stored for a long period of time, the gel strength gradually decreases, and sufficient ink backflow prevention performance cannot be obtained, causing problems such as leaving the chip upward (upright) or ink leakage due to impact. There was a risk of occurrence.
本発明は従来のインキ逆流防止体の不具合を解消するものであって、インキ成分との親和性の高いベースオイルを使用しても、インキとインキ逆流防止体の相互作用によるインキ逆流防止体或いはインキの劣化、変質、変色等が発生せず、しかも、剪断力や長期保存による物性の変化が少なく、インキ追従性とインキ逆流防止性能に優れたインキ逆流防止体の製造方法を提供しようとするものである。
尚、本発明において「前」とはペン先側を、「後」とはインキ逆流防止体側を指し、また「正立」とはペン先を上向き、「倒立」とはペン先を下向き状態にすることを示す。
The present invention solves the problems of the conventional ink backflow prevention body, and even if a base oil having a high affinity with the ink component is used, the ink backflow prevention body or ink by the interaction between the ink and the ink backflow prevention body It is intended to provide a method for producing an ink backflow prevention body that does not cause deterioration, deterioration, discoloration, etc., has little change in physical properties due to shearing force or long-term storage, and has excellent ink followability and ink backflow prevention performance. It is.
In the present invention, “front” refers to the pen tip side, “rear” refers to the ink backflow preventer side, “upright” refers to the pen tip upward, and “inverted” refers to the pen tip downward. Indicates to do.
本発明者は種々のベースオイルと増粘剤を組み合わせ、インキ追従性とインキ逆流防止性能を同時に満足し、更に衝撃或いは長期間の保存によっても初期の性能を維持することができるインキ逆流防止体を検討した結果、本発明を完成するに至った。 The present inventor combined various base oils and thickeners to provide an ink backflow prevention body that satisfies ink followability and ink backflow prevention performance at the same time, and can maintain the initial performance even after impact or long-term storage. As a result of the study, the present invention has been completed.
即ち、本発明は筆記具のインキ収容筒内に直接収容したインキの後端面に配設され、インキの消費に従い前進するインキ逆流防止体の製造方法であって、下記一般式（１）で示される脂肪酸アマイドを予め芳香族炭化水素、脂環族炭化水素、ケトン及び低級脂肪族アルコールから選ばれる一種又は二種以上の有機溶媒に溶解或いは膨潤させた後、エチレン−α−オレフィンコオリゴマー、α−オレフィン油、精製鉱油及びポリブテンから選ばれる一種又は二種以上と混合することを特徴とする筆記具用インキ逆流防止体組成物の製造方法を要件とする。
本発明の製造方法で得られるインキ逆流防止体組成物は、インキ逆流防止体に要求されるインキ追従性とインキ逆流防止性の相反する二つの重要な特性を同時に満足し、更に長期の保管においても硬さの変化や基油の分離等が発生しないという特徴を有する。また、インキ収容管に充填する工程等で剪断力を付加された場合も顕著な粘度低下がなく、剪断力が取り去られた後は速やかに元の粘度に復元するため、筆記具の製造工程においても、インキ漏れ等の不具合が発生することがない。 The ink backflow preventive body composition obtained by the production method of the present invention simultaneously satisfies the two important characteristics of the ink followability and ink backflow prevention required for the ink backflow preventive body, and further, for long-term storage. Has the characteristic that no change in hardness or separation of the base oil occurs. In addition, when shearing force is applied in the process of filling the ink containing tube, etc., there is no significant decrease in viscosity, and after the shearing force is removed, the original viscosity is quickly restored. However, problems such as ink leakage do not occur.
本発明においてベースオイルとして用いられる難揮発性溶剤は、エチレン−α−オレフィンコオリゴマー、α−オレフィン油、精製鉱油及びポリブテンから一種又は二種以上が選ばれる。 In the present invention, the hardly volatile solvent used as the base oil is selected from ethylene-α-olefin co-oligomer, α-olefin oil, refined mineral oil, and polybutene.
また増粘剤として添加される脂肪酸アマイドは前記一般式（１）で表わされる化合物であり、一般式（１）で示される化合物で式中のＲ２が水素である化合物の具体例としてはラウリン酸アマイド、ステアリン酸アマイド、オレイン酸アマイド、エルカ酸アマイド、リシノール酸アマイド、１２−ヒドロキシステアリン酸アマイド等を挙げることができる。また、式中のＲ２がアルキル基或いはアルケニル基である化合物の具体例としてはＮ−イソブチルラウリン酸アマイド、Ｎ−イソブチルステアリン酸アマイド、Ｎ−オレイルステアリン酸アマイド、Ｎ−オレイルオレイン酸アマイド、Ｎ−ステアリルステアリン酸アマイド、Ｎ−ステアリルオレイン酸アマイド、Ｎ−オレイルパルミチン酸アマイド、Ｎ−ステアリルエルカ酸アマイド等を挙げることができる。 The fatty acid amide to be added as a thickener is a compound represented by the general formula (1), lauric Specific examples of compounds in which R 2 is hydrogen wherein a compound represented by the general formula (1) Examples thereof include acid amide, stearic acid amide, oleic acid amide, erucic acid amide, ricinoleic acid amide and 12-hydroxystearic acid amide. Specific examples of the compound in which R 2 in the formula is an alkyl group or an alkenyl group include N-isobutyl lauric acid amide, N-isobutyl stearic acid amide, N-oleyl stearic acid amide, N-oleyl oleic acid amide, N -Stearyl stearic acid amide, N-stearyl oleic acid amide, N-oleyl palmitic acid amide, N-stearyl erucic acid amide etc. can be mentioned.
更に、一般式（１）で示される化合物で式中のＲ２がシクロアルキル置換アルキル基である化合物としては、Ｎ−シクロヘキシルメチルラウリン酸アマイド、Ｎ−シクロヘキシルメチルカプロン酸アマイド等が例示できる。 Furthermore, examples of the compound represented by the general formula (1) in which R 2 is a cycloalkyl-substituted alkyl group include N-cyclohexylmethyl lauric acid amide and N-cyclohexylmethyl caproic acid amide.
これらの脂肪酸アマイドの一種又は二種以上をインキ逆流防止体全量に対して０．２〜３．０重量％添加することにより本発明のインキ逆流防止体組成物を得ることができる。添加量が０．２重量％未満では得られるインキ逆流防止体の粘度が十分ではなく、正立放置によりインキ逆流防止体がインキ収容管の後端方向に移動する、或いは正立状態で筆記具を落下させた時にインキ逆流防止体やインキが流出或いは飛散してしまう等の不具合を生じることもある。 The ink backflow preventer composition of the present invention can be obtained by adding 0.2 to 3.0% by weight of one or more of these fatty acid amides with respect to the total amount of the ink backflow preventer. If the amount added is less than 0.2% by weight, the viscosity of the ink backflow preventive body obtained is not sufficient, and the ink backflow preventive body moves toward the rear end of the ink storage tube when left standing upright, or the writing instrument is placed in the upright state. In some cases, the ink backflow prevention body or ink may flow out or scatter when dropped.
また、前記脂肪酸アマイドの添加量が３重量％を超えると、得られるインキ逆流防止体が硬くなりすぎるために、筆記時にインキの消費と共にペン体方向への追従が阻害され、インキの供給が不足し、筆跡濃度低下や筆記線途切れ等が発生することもある。
前記脂肪酸アマイドは０．２〜３．０重量％の添加量が好ましいが、０．５〜２．０重量％の添加がより好ましい。
Also, if the amount of fatty acid amide added exceeds 3% by weight, the resulting ink backflow preventive body becomes too hard, which obstructs follow-up in the direction of the pen body as ink is consumed during writing, and ink supply is insufficient. In some cases, however, handwriting density drop or writing line interruption may occur.
The fatty acid amide is preferably added in an amount of 0.2 to 3.0% by weight, more preferably 0.5 to 2.0% by weight.
本発明のインキ逆流防止体組成物の主成分は前述したようにエチレン−α−オレフィンコオリゴマー、α−オレフィン油、精製鉱油及びポリブテンから選ばれる一種又は二種以上と前記脂肪酸アマイドであるが、更にゲル強度を増すために従来からインキ逆流防止体組成物の増粘剤として汎用されている微粒子シリカ（親水性或いは疎水性）、ベンジリデンソルビトール類、アミノ酸誘導体ベントナイト、膨潤性雲母等を補助増粘剤として少量添加することも有効である。
また、粘度調整剤としてアタクチックポリプロピレン或いはエチレン−α−オレフィン樹脂を添加してもよい。
As described above, the main component of the ink backflow preventive composition of the present invention is one or more selected from ethylene-α-olefin co-oligomer, α-olefin oil, refined mineral oil and polybutene and the fatty acid amide. In order to further increase the gel strength, auxiliary thickeners such as fine-particle silica (hydrophilic or hydrophobic), benzylidene sorbitols, amino acid derivative bentonite, and swellable mica, which have been widely used as thickeners in ink backflow preventive compositions, have been used. It is also effective to add a small amount as an agent.
Moreover, you may add an atactic polypropylene or ethylene-alpha-olefin resin as a viscosity modifier.
本発明のインキ逆流防止体組成物に用いられる脂肪酸アマイドは、ベースオイルとして用いられるエチレン−α−オレフィンコオリゴマー、α−オレフィン油、精製鉱油或いはポリブテンとの相溶性が低いために、単純な攪拌のみでは良好な分散体を得ることは困難である。よって、予め脂肪酸アマイドをキシレン、ミネラルターペン、メチルイソブチルケトン、エチルアルコール等の低沸点溶剤に１０〜２０重量％の濃度で加温溶解或いは膨潤させたペーストを作成し、ベースオイル中に所定量の前記脂肪酸アマイドペーストを投入し、ディスパー等で予備攪拌したものを三本ロールで分散処理する製造方法が好適である。尚、ペースト作成に使用した低沸点溶媒は、三本ロール処理が開放状態で行なわれるため、分散処理終了までに揮散する。 Since the fatty acid amide used in the ink backflow preventive composition of the present invention has low compatibility with the ethylene-α-olefin co-oligomer, α-olefin oil, refined mineral oil or polybutene used as the base oil, only simple stirring is required. Thus, it is difficult to obtain a good dispersion. Therefore, a paste in which fatty acid amide is preliminarily dissolved or swollen in a low-boiling solvent such as xylene, mineral terpene, methyl isobutyl ketone, and ethyl alcohol at a concentration of 10 to 20% by weight is prepared, and a predetermined amount of the above-described amount is added to the base oil. A production method in which a fatty acid amide paste is charged and pre-stirred with a disper or the like is dispersed with a three-roll machine is suitable. Note that the low boiling point solvent used for preparing the paste is volatilized by the end of the dispersion process because the three-roll process is performed in an open state.
前記低沸点溶剤は、用いられる脂肪酸アマイドに対する溶解力の高いものが選択されるが、具体的にはミネラルターペン等の脂肪族炭化水素、トルエン、キシレン等の芳香族炭化水素、メチルエチルケトン、メチルイソブチルケトン等のケトン類、エチルアルコール、イソプロピルアルコール、ｎ−ブチルアルコール等の低級アルコール及び酢酸エチル、酢酸ブチル等のエステル類等から選ばれる一種又は二種以上の混合溶剤が使用される。
選択された単独或いは混合溶剤中に脂肪酸アマイドを全体の１０〜２０重量％の範囲で投入し、環流冷却器を備えたフラスコ中で７５〜１２０℃の温度で均一になるまで攪拌することにより、脂肪酸アマイドペーストが得られる。
The low boiling point solvent is selected from those having high solubility in the fatty acid amide used, specifically, aliphatic hydrocarbons such as mineral terpenes, aromatic hydrocarbons such as toluene and xylene, methyl ethyl ketone, methyl isobutyl ketone. One or two or more mixed solvents selected from ketones such as ethyl alcohol, isopropyl alcohol, lower alcohols such as n-butyl alcohol, and esters such as ethyl acetate and butyl acetate are used.
Into the selected single or mixed solvent, the fatty acid amide is charged in the range of 10 to 20% by weight of the whole, and stirred in a flask equipped with a reflux condenser at a temperature of 75 to 120 ° C. until uniform. A fatty acid amide paste is obtained.
前記脂肪酸アマイドペーストとベースオイルとして用いられるエチレン−α−オレフィンコオリゴマー、α−オレフィン油、精製鉱油及びポリブテンから選ばれる一種又は二種以上を所定量混合して予備攪拌をした後、三本ロール処理をすることにより本発明のインキ逆流防止体組成物を得ることができる。
前記製造方法で作成することにより、脂肪酸アマイドはベースオイル中に均一な微粒子状態に分散され、微細な三次元網目構造を形成する。そのため、高揺変性を有し、また剪断力が付加されたときも急激な粘度低下を示さず、更には、長期間保管された場合も油分の分離等が発生せず経時的に安定なゲル状態が保持され、良好なインキ逆流防止体が得られる。
Three-roll treatment after pre-stirring by mixing a predetermined amount of one or more selected from the fatty acid amide paste and ethylene-α-olefin co-oligomer, α-olefin oil, refined mineral oil and polybutene used as base oil By doing so, the ink backflow preventive composition of the present invention can be obtained.
By producing by the said manufacturing method, a fatty acid amide is disperse | distributed in a uniform fine particle state in base oil, and forms a fine three-dimensional network structure. Therefore, it has a high thixotropic property and does not show a drastic drop in viscosity even when a shearing force is applied. Furthermore, even when stored for a long period of time, it does not cause separation of oil and is stable over time. The state is maintained, and a good ink backflow preventer is obtained.
以下、本発明の筆記具用インキ逆流防止体組成物の実施例と比較例を説明するが、本発明はこれらの実施例に限定されるものではない。 Hereinafter, examples and comparative examples of the ink backflow preventive composition for a writing instrument of the present invention will be described, but the present invention is not limited to these examples.
〔脂肪酸アマイドペーストの作成〕
脂肪酸アマイドペーストＡ
エチルアルコール１５重量部、キシロール６５重量部、Ｎ−シクロヘキシルメチルラウリン酸アマイド２０重量部を環流冷却器を備えたフラスコ中に投入し、１０５℃で均一になるまで攪拌した後、室温で放冷し脂肪酸アマイドペーストＡを得た。
脂肪酸アマイドペーストＢ
ミネラルスピリット９０重量部、Ｎ−イソブチルラウリン酸アマイド１０重量部を環流冷却器を備えたフラスコ中に投入し、１２０℃で均一になるまで攪拌した後、室温で放冷し、脂肪酸アマイドペーストＢを得た。
脂肪酸アマイドペーストＣ
エチルアルコール２５重量部、キシロール６５重量部、Ｎ−ステアリルステアリン酸アマイド１０重量部を環流冷却器を備えたフラスコ中に投入し、１０５℃で均一になるまで攪拌した後、室温で放冷し、脂肪酸アマイドペーストＣを得た。
[Creation of fatty acid amide paste]
Fatty acid amide paste A
15 parts by weight of ethyl alcohol, 65 parts by weight of xylol and 20 parts by weight of N-cyclohexylmethyl lauric acid amide were put into a flask equipped with a reflux condenser, stirred at 105 ° C. until uniform, and then allowed to cool at room temperature. Fatty acid amide paste A was obtained.
Fatty acid amide paste B
90 parts by weight of mineral spirits and 10 parts by weight of N-isobutyl lauric acid amide are put into a flask equipped with a reflux condenser, stirred at 120 ° C. until uniform, and then allowed to cool at room temperature to obtain fatty acid amide paste B. Obtained.
Fatty acid amide paste C
25 parts by weight of ethyl alcohol, 65 parts by weight of xylol and 10 parts by weight of N-stearyl stearic acid amide were put into a flask equipped with a reflux condenser, stirred at 105 ° C. until uniform, and then allowed to cool at room temperature. Fatty acid amide paste C was obtained.
実施例及び比較例のインキ逆流防止体組成物の配合を以下の表に示す。表中の数字は重量部を表わす。
尚、実施例及び比較例１、２はベースオイル中に脂肪酸アマイドペーストを所定量投入し、予備攪拌をした後三本ロール処理を行ないインキ逆流防止体を得た。
また、比較例３から６についてはベースオイル中にゲル化剤を所定量投入、ディスパーで攪拌しながら加温し、１４０℃になった時点で攪拌及び加温を停止し、室温まで自然放冷することによりインキ逆流防止体を得た。
得られた実施例及び比較例のインキ逆流防止体の硬さを平行板粘度計（スプレッドメーター）で測定した値をＳＭ値の欄に記載した。
但し、比較例５はゲル化剤による増粘ができず、ベースオイルと同程度の粘度であったため平行板粘度計の測定及び性能試験の対象から除外した。
The formulation of the ink backflow preventive compositions of Examples and Comparative Examples is shown in the following table. The numbers in the table represent parts by weight.
In Examples and Comparative Examples 1 and 2, a predetermined amount of fatty acid amide paste was added to the base oil, and after pre-stirring, a three-roll treatment was performed to obtain an ink backflow preventer.
For Comparative Examples 3 to 6, a predetermined amount of gelling agent was added to the base oil and heated while stirring with a disper. When the temperature reached 140 ° C., the stirring and heating were stopped and the mixture was allowed to cool to room temperature. As a result, an ink backflow preventer was obtained.
The values obtained by measuring the hardness of the obtained ink backflow preventers of Examples and Comparative Examples with a parallel plate viscometer (spread meter) are shown in the SM value column.
However, since Comparative Example 5 could not be thickened with a gelling agent and had a viscosity comparable to that of the base oil, it was excluded from the parallel plate viscometer measurement and performance test.
表中の原料を注番号に従って説明する。
（１）ポリブテン３ＳＨ〔日本油脂（株）製、液状ポリブテン、平均分子量：７２０、粘度２１００ｃＳｔ（４０℃）〕
（２）ルーカントＨＣ−１５０〔三井石油化学（株）製、エチレン−α−オレフィン−コオリゴマー、粘度２２００ｃＳｔ（４０℃）〕
（３）ゲルオールＤ〔新日本理化（株）製、ジベンジリデンソルビトール〕
（４）ＧＰ−１〔味の素（株）製、アシル化アミノ酸〕
The raw materials in the table will be described according to the note numbers.
(1) Polybutene 3SH [manufactured by NOF Corporation, liquid polybutene, average molecular weight: 720, viscosity 2100 cSt (40 ° C.)]
(2) Lucant HC-150 [Mitsui Petrochemical Co., Ltd., ethylene-α-olefin-co-oligomer, viscosity 2200 cSt (40 ° C.)]
(3) Gelol D [Shin Nihon Rika Co., Ltd., Dibenzylidene Sorbitol]
(4) GP-1 [Ajinomoto Co., Inc., acylated amino acid]
試料ボールペンの作製
０．７ｍｍ径の超硬合金製ボールを備えたステンレスパイプチップを先端に嵌着した、内径３．８ｍｍのポリエチレン管に、２０℃における粘度が１００ｍＰａ・ｓの水性黒インキを充填しインキ後端部に実施例及び比較例のインキ逆流防止体組成物をそれぞれ接触配置して試料ボールペンとし、以下の性能試験を行なった。
Preparation of sample ballpoint pen Filled with 3.8mm inner diameter polyethylene tube with stainless steel pipe tip with 0.7mm diameter cemented carbide ball tip, water-based black ink with viscosity at 20 ° C of 100mPa · s The ink backflow preventive compositions of Examples and Comparative Examples were placed in contact with the rear end of the ink and used as sample ballpoint pens, and the following performance tests were performed.
〔逆流試験〕
前記試料ボールペンを、正立状態のまま４フィートの高さから落下し、インキ逆流防止体の状態を目視で観察した。
〔追従性試験〕
前記試料ボールペンを筆記荷重１００ｇ、筆記速度１０ｍ／分の条件で筆記試験を行なった。
〔耐剪断力試験〕
実施例及び比較例のインキ逆流防止体をディスパーを用いて１５００ｒｐｍで５分間攪拌した直後に前記の部品及びインキを用いてボールペンを組み立て、前記と同様の逆流試験を行なった。
〔基油分離試験〕
前記試料ボールペンを、正立状態で５０℃雰囲気に一カ月放置した後、インキ逆流防止体の状態を目視で観察した。
[Backflow test]
The sample ball-point pen was dropped from a height of 4 feet in an upright state, and the state of the ink backflow preventer was visually observed.
[Followability test]
The sample ball-point pen was subjected to a writing test under the conditions of a writing load of 100 g and a writing speed of 10 m / min.
[Shear resistance test]
Immediately after stirring the ink backflow prevention bodies of Examples and Comparative Examples using a disper at 1500 rpm for 5 minutes, a ballpoint pen was assembled using the above components and ink, and a backflow test similar to the above was performed.
[Base oil separation test]
The sample ballpoint pen was left in an upright state at 50 ° C. for one month, and then the state of the ink backflow preventer was visually observed.
上記の試験を行なった結果を以下の表に示す。尚、それぞれの試験における評価基準は以下の通りである。
〔逆流試験〕
○：インキ逆流防止体の状態に変化が認められない。
△：インキ逆流防止体の形状が崩れている。
×：インキ逆流防止体の形状が崩れ、インキが後方に漏出している。
〔追従性試験〕
○：良好に筆記できる。
△：筆記線にカスレが発生している。
×：筆記線が途切れる。或いは筆記できない。
〔耐剪断力試験〕
○：インキ逆流防止体の状態に変化が認められない。
△：インキ逆流防止体の形状が崩れている。
×：インキ逆流防止体の形状が崩れ、インキが後方に漏出している。
〔基油分離試験〕
○：インキ逆流防止体の状態に変化が認められない。
△：インキ逆流防止体の一部が分離し、インキ中に移行している。
×：インキ逆流防止体の一部が分離し、ペン先まで移行している。
The following table shows the results of the above tests. In addition, the evaluation criteria in each test are as follows.
[Backflow test]
○: No change is observed in the state of the ink backflow preventer.
Δ: The shape of the ink backflow preventer is broken.
X: The shape of the ink backflow preventer is broken, and the ink leaks backward.
[Followability test]
○: Can be written well.
Δ: Scratch occurs on the writing line.
X: The writing line is interrupted. Or I can't write.
[Shear resistance test]
○: No change is observed in the state of the ink backflow preventer.
Δ: The shape of the ink backflow preventer is broken.
X: The shape of the ink backflow preventer is broken, and the ink leaks backward.
[Base oil separation test]
○: No change is observed in the state of the ink backflow preventer.
(Triangle | delta): A part of ink backflow prevention body isolate | separated and it has moved in the ink.
X: A part of the ink backflow preventer is separated and is transferred to the pen tip.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2009119403A JP4861543B2 (en) | 2009-05-18 | 2009-05-18 | Method for producing ink backflow preventive composition for writing instrument |
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| Application Number | Priority Date | Filing Date | Title |
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| JP2009119403A JP4861543B2 (en) | 2009-05-18 | 2009-05-18 | Method for producing ink backflow preventive composition for writing instrument |
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| JP2000175110A Division JP4510995B2 (en) | 2000-06-12 | 2000-06-12 | Ink backflow preventive composition for writing instruments |
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| JP4861543B2 true JP4861543B2 (en) | 2012-01-25 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS57200472A (en) * | 1981-06-04 | 1982-12-08 | Sakura Color Prod Corp | Back-flow preventing composition for writing ink |
| JP3505660B2 (en) * | 1993-03-11 | 2004-03-08 | パイロットインキ株式会社 | Writing implement ink backflow prevention body |
| JP2000043465A (en) * | 1998-07-30 | 2000-02-15 | Pilot Corp | Oleaginous ball-point pen |
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