JP5396209B2 - Synthetic rubber base anti-adhesive composition and method - Google Patents
Synthetic rubber base anti-adhesive composition and method Download PDFInfo
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Description
本発明は、合成ゴム基材、例えばゴムシートの防着剤組成物および防着方法に関する。ここで術語「防着」とは、二つの物体の露出面を接触させた時、接触によって生じた凝集力あるいは付着力により、引張力を加えれば分離可能であるが、半永久的に離れなくなるスティッキングを防止することを意味する。 The present invention relates to an anti-adhesive composition and an anti-adhesion method for a synthetic rubber substrate such as a rubber sheet. Here, the term “adhesion” means sticking that can be separated by applying a tensile force due to the cohesive force or adhesive force generated by the contact when the exposed surfaces of two objects are brought into contact, but cannot be separated semipermanently. Means to prevent.
ゴム、プラスチックなどの多数のシートを積層する場合、スティッキングにより一枚毎の取出しに支障を来す場合がある。また連続シートをロールに巻いて貯蔵する場合などでもスティッキングは巻き戻しに支障を来たす。スティッキングを防止する方法として打粉と呼ばれるタルク、炭酸カルシウム等の粉体を表面に撒布する方法、金属石鹸やシリコーンオイルなどの離型性を有する材料を塗布する方法、表面を艶消し仕上げ(マット仕上げ)する方法などが知られている。これらの方法は、シートの材質、用途、半製品か完成品かの区別、所望の効果持続性、コスト等によって適用できない場合がある。 When a large number of sheets such as rubber and plastic are stacked, sticking may hinder the removal of each sheet. Sticking also hinders rewinding even when a continuous sheet is wound on a roll and stored. As a method to prevent sticking, talc, which is called dusting, a method of spreading powder such as calcium carbonate on the surface, a method of applying a releasable material such as metal soap or silicone oil, matte finish (matte finish) ) Is known. These methods may not be applied depending on the material of the sheet, the application, the distinction between a semi-finished product and a finished product, desired effect durability, cost, and the like.
特許第3478383号公報(特許文献1)は、特定の熱可塑性エラストマーの成形体に、平均粒径が500μm以下のポリオレフィンを主成分とする粒状物質を付着させることによってスティッキングを防止する方法を開示している。この場合のスティッキング防止効果は、タルク等の無機粉末の打粉に代えてポリオレフィン粉末を用いるという違いはあるにせよ原理的には同じである。 Japanese Patent No. 3478383 (Patent Document 1) discloses a method for preventing sticking by adhering a granular material mainly composed of polyolefin having an average particle diameter of 500 μm or less to a specific thermoplastic elastomer molded body. ing. In this case, the sticking prevention effect is the same in principle, although there is a difference that a polyolefin powder is used instead of the dusting of an inorganic powder such as talc.
打粉またはこれに代るポリオレフィンパウダー等の撒布は、付着させた成形品から飛散し易いこと、粉塵の発生を避けるため成形体への付着は防塵施設を必要とすること、成形体が濃く着色されている場合、白いかすみがかった外観を呈することなどの欠点を有する。このため上記欠点のないゴム、プラスチック製、特に合成ゴム製の成形シートの防着剤組成物および防着方法の提供が望まれる。 Dispersion such as dusting or alternative polyolefin powder is easy to scatter from the attached molded product, adherence to the molded product requires a dust-proof facility to avoid generation of dust, and the molded product is darkly colored. If so, it has drawbacks such as a white hazy appearance. Therefore, it is desired to provide an anti-adhesive composition and an anti-adhesion method for molded sheets made of rubber, plastic, particularly synthetic rubber, which do not have the above drawbacks.
本発明は、水中で可逆的に剥離する改質Mg−Al型層状複水酸化物の水分散液よりなることを特徴とする合成ゴムシート用スティッキング防止剤組成物を提供する。 The present invention provides an anti-sticking composition for a synthetic rubber sheet comprising an aqueous dispersion of a modified Mg—Al type layered double hydroxide that reversibly peels in water.
改質Mg−Al型層状複水化物は、
式:Mg1−xAlx(OH)2(式中、xは0.2ないし0.33である。)を有する隣接する複数の基本複水酸化物層の間に、水溶性脂肪族モノカルボン酸マグネシウムと層間水がインターカレーションにより取込まれた化合物である。
The modified Mg-Al type layered double hydrate is
Between adjacent basic double hydroxide layers having the formula: Mg 1-x Al x (OH) 2 , where x is 0.2 to 0.33, water-soluble aliphatic mono This is a compound in which magnesium carboxylate and interlayer water are incorporated by intercalation.
この改質Mg−Al型層状複水酸化物を水に投ずると、層間で剥離してナノサイズのシート状粒子のゾルとなる。これを例えば金属に塗装し、乾燥すると透明な基材に密着した皮膜を形成する。このため、本発明の防着剤組成物を防着を必要とするシート、特に合成ゴムシートに塗布し、乾燥して皮膜を形成することにより、シートの防着を達成することができる。 When this modified Mg—Al-type layered double hydroxide is poured into water, it peels between the layers to form a sol of nano-sized sheet-like particles. When this is applied to, for example, a metal and dried, a film that adheres to a transparent substrate is formed. For this reason, the adhesion prevention of a sheet | seat can be achieved by apply | coating the anti-adhesive agent composition of this invention to the sheet | seat which needs adhesion, especially a synthetic rubber sheet, and drying and forming a film | membrane.
防着は積層した多数の合成ゴムシートまたはシートを巻取ったロールに有効であるばかりでなく、合成ゴムシートと、他の材質のシート状物体との防着にも有効である。この場合、隣接する合成ゴムシート間の防着のためにはシートの片面にだけ防着剤組成物を塗布すればよく、合成ゴムシートと他の材質のシート状物体の場合は合成ゴムシートの接触面だけに防着剤組成物を塗布すればよい。 The adhesion is effective not only for a large number of laminated synthetic rubber sheets or rolls wound with the sheets, but also for adhesion between the synthetic rubber sheets and sheet-like objects of other materials. In this case, in order to prevent adhesion between adjacent synthetic rubber sheets, it is only necessary to apply the anti-adhesive composition on one side of the sheet. In the case of a synthetic rubber sheet and a sheet-like object of another material, the synthetic rubber sheet The anti-adhesive composition may be applied only to the contact surface.
本発明の防着剤組成物は、打粉およびこれと原理を同じくする粉体粒子に比較していくつかの利点を有する。それらは、i)シート表面に連続した皮膜を形成するから取扱いによって飛散しないこと、ii)皮膜は透明であるためシートの外観に影響しないこと、iii)水分散液のため粉塵対策が必要でないこと、iv)乾燥した粉体の形で提供され、現場で水を加えて分散液に調製されるので、分散液の濃度を変えることによって塗布方法(スプレー、刷毛塗り、ローラー、ディッピング等)に適した粘度に調節することができ、必要な場合は他の添加剤を添加することができることを含む。 The anti-adhesive composition of the present invention has several advantages over powdered powder and powder particles similar in principle. They are: i) a continuous film is formed on the surface of the sheet, so that it does not scatter by handling, ii) the film is transparent and does not affect the appearance of the sheet, and iii) no dust measures are required for the aqueous dispersion. Iv) Provided in the form of dry powder and prepared in dispersion by adding water on site, suitable for application methods (spray, brushing, roller, dipping, etc.) by changing the concentration of the dispersion The viscosity can be adjusted and other additives can be added if necessary.
A.改質Mg−Al型層状複水酸化物
水中で可逆的に剥離する改質Mg−Al型層状複水酸化物は、式
Mg1−xAlx(OH)2
(式中、xは0.2〜0.33)を有する複数の基本層の間に、水溶性脂肪族モノカルボン酸マグネシウム塩と層間水がインターカレーションにより取り込まれている化合物である。脂肪族モノカルボン酸マグネシウム塩の例は、酢酸マグネシウム、乳酸マグネシウム、アクリル酸マグネシウムなどである。
A. Modified Mg—Al-type layered double hydroxide The modified Mg—Al-type layered double hydroxide that reversibly peels off in water has the formula Mg 1-x Al x (OH) 2
(Wherein x is 0.2 to 0.33) is a compound in which a water-soluble aliphatic monocarboxylic acid magnesium salt and interlayer water are incorporated by intercalation between a plurality of basic layers. Examples of the aliphatic monocarboxylic acid magnesium salt include magnesium acetate, magnesium lactate, and magnesium acrylate.
このものの製造法は、例えば本出願人のWO2006/068118公報に記載されており、Mg−Al炭酸型層状複水酸化物(以後「層状複水酸化物」を「LDH」と略す。)、
式:〔Mg1−xAlx(OH)2〕〔(CO3)x/2・yH2O〕
のハイドロタルサイトから出発する。ハイドロタルサイトおよびその他の炭酸型LDH自体は水中で剥離しない。改質は、このハイドロタルサイトを400℃〜800℃の温度で焼成し、炭酸イオンの大部分を除去した熱分解物を、水溶性の脂肪族モノカルボン酸のマグネシウム塩と水中において反応させて行う。反応生成物は一般にゲル状の固体である。この固体を反応混合物から分離し、好ましくは100℃までの温度で乾燥し、粉砕すれば、水中で可逆的に剥離してナノサイズの粒子のゾルを形成する改質Mg−Al型LDHが得られる。
A manufacturing method of this is described in, for example, the applicant's WO 2006/068118, and Mg—Al carbonate type layered double hydroxide (hereinafter, “layered double hydroxide” is abbreviated as “LDH”),
Formula: [Mg 1-x Al x (OH) 2 ] [(CO 3 ) x / 2 · yH 2 O]
Starting from hydrotalcite. Hydrotalcite and other carbonated LDH itself do not exfoliate in water. In the modification, the hydrotalcite is calcined at a temperature of 400 ° C. to 800 ° C., and a pyrolyzate from which most of carbonate ions have been removed is reacted with a water-soluble magnesium salt of an aliphatic monocarboxylic acid in water. Do. The reaction product is generally a gel-like solid. If this solid is separated from the reaction mixture, preferably dried at a temperature of up to 100 ° C. and pulverized, a modified Mg-Al type LDH is obtained that reversibly peels in water to form a sol of nano-sized particles. It is done.
B.防着剤組成物
本発明の防着剤組成物は、前節Aで説明した改質LDHを所望の固形分濃度、例えば0.5%、1%、2%、3%等の水に分散することによって調製される。この分散液はナノサイズのシート状粒子のゾルを形成し、固形分濃度に比例して粘度が高くなるので、塗装方法に適した粘度の固形分濃度とする必要がある。一般に3%より高い固形分濃度は好ましくない。単独で皮膜を形成するのでバインダーとして水溶性フィルム形成ポリマーを添加する必要はない。ただし、消泡剤などの添加は任意である。
B. Antiadhesive Composition The antiadhesive composition of the present invention disperses the modified LDH described in the preceding section A in water at a desired solid content, for example, 0.5%, 1%, 2%, 3%, etc. It is prepared by. Since this dispersion forms a sol of nano-sized sheet-like particles and the viscosity increases in proportion to the solid content concentration, it is necessary to make the solid content concentration suitable for the coating method. In general, solids concentrations higher than 3% are not preferred. Since a film is formed alone, it is not necessary to add a water-soluble film-forming polymer as a binder. However, addition of an antifoaming agent etc. is arbitrary.
C.防着皮膜の形成方法
本発明の防着剤組成物は、防着を必要とするシートのような合成ゴム基材へ塗装し、乾燥することにより防着機能を有する皮膜を形成する。中でも基材の材質がポリオレフィン系熱可塑性エラストマー、例えばエチレン−プロピレンゴム(EPM,EPDM)、ニトリルゴム(NBR)、ポリスチレン系熱可塑製エラストマー、例えばスチレン、ブタジエン、スチレンのトリブロック共重合体の水素化物、クロロプレン、およびシリコーンゴムであるシート状基材が防着を特に必要とする基材の例である。この他、タルクなどの打粉が使用される多層電線の熱融着防止剤としても利用できる。
C. Method for Forming an Adhesive Film The antiadhesive composition of the present invention forms a film having an antiadhesive function by coating on a synthetic rubber substrate such as a sheet that requires anti-adhesion and drying. Among them, the material of the base material is a polyolefin-based thermoplastic elastomer such as ethylene-propylene rubber (EPM, EPDM), nitrile rubber (NBR), polystyrene-based thermoplastic elastomer such as styrene, butadiene, hydrogen of a triblock copolymer of styrene. Sheet-like substrates that are chemicals, chloroprene, and silicone rubber are examples of substrates that particularly require adhesion. In addition, it can also be used as a heat fusion preventive agent for multilayer electric wires in which dusting powder such as talc is used.
塗装方法は、スプレー、バーコーター、刷毛塗り、ローラー塗装、ディッピング等の慣用塗装方法でよい。塗装後室温または100℃までの温度で乾燥し、皮膜を形成させる。単位面積あたり同じ塗布量で防着剤組成物の皮膜を形成させた場合、固形分濃度に比例して乾燥膜厚が厚くなり、皮膜が可撓性を失う。そのため3%以上の固形分濃度を避けるか、または単位面積あたりの塗布量を少なくして皮膜の可撓性を保持するのが好ましい。 The coating method may be a conventional coating method such as spraying, bar coater, brush coating, roller coating or dipping. After coating, the film is dried at room temperature or up to 100 ° C. to form a film. When a film of the antiadhesive composition is formed at the same coating amount per unit area, the dry film thickness increases in proportion to the solid content concentration, and the film loses flexibility. Therefore, it is preferable to avoid the solid content concentration of 3% or more, or to keep the flexibility of the film by reducing the coating amount per unit area.
改質LDHにインターカレートされるマグネシウム塩としてアクリル酸マグネシウムを選択した場合、皮膜を紫外線で照射することによってアクリル酸マグネシウムを架橋重合し、皮膜の耐水性を高めることができる。紫外線の代わりに電子線を照射することによっても架橋重合は可能である。 When magnesium acrylate is selected as the magnesium salt intercalated with the modified LDH, the magnesium acrylate can be crosslinked and polymerized by irradiating the film with ultraviolet rays, thereby increasing the water resistance of the film. Cross-linking polymerization is also possible by irradiating an electron beam instead of ultraviolet rays.
以下の実施例は例証目的であって、本発明を限定することを意図しない。実施例中、%は重量基準による。 The following examples are for illustrative purposes and are not intended to limit the invention. In the examples,% is based on weight.
第1部 再構築(改質)LDHの製造
製造例1
(a)Mg−Al炭酸型LDH(協和化学工業(株)製DHT−6)を700℃において20時間加熱して熱分解物を得た。
(b)この熱分解物96.3gを酢酸マグネシウム・4水塩0.28mol/L(60g/L)水溶液1Lへ加え、室温で15時間攪拌した後、生成した固体(ゲル)を濾過して分離し、90℃で10時間乾燥し、粉砕して酢酸マグネシウムがインターカレートされた再構築(改質)LDHを得た。このものをLDH I−1と呼ぶ。
Part 1 Production of reconstructed (modified) LDH Production Example 1
(a) Mg-Al carbonate type LDH (DHT-6 manufactured by Kyowa Chemical Industry Co., Ltd.) was heated at 700 ° C. for 20 hours to obtain a thermal decomposition product.
(b) 96.3 g of this pyrolyzate was added to 1 L of a magnesium acetate tetrahydrate 0.28 mol / L (60 g / L) aqueous solution and stirred at room temperature for 15 hours, and then the resulting solid (gel) was filtered. Separated, dried at 90 ° C. for 10 hours, and ground to obtain a reconstructed (modified) LDH in which magnesium acetate was intercalated. This is called LDH I-1.
製造例2
酢酸マグネシウムをアクリル酸マグネシウムに変更する以外は製造例1と同様の操作を行い、アクリル酸マグネシウムがインターカレートされた再構築(改質)LDHを得た。このものをLDH I−2と呼ぶ。
Production Example 2
Except for changing magnesium acetate to magnesium acrylate, the same operation as in Production Example 1 was performed to obtain a reconstructed (modified) LDH in which magnesium acrylate was intercalated. This is called LDH I-2.
製造例3
酢酸マグネシウムを乳酸マグネシウムに変更する以外は製造例1と同様の操作を行い、乳酸マグネシウムがインターカレートされた再構築(改質)LDHを得た。このものをLDH I−3と呼ぶ。
Production Example 3
Except for changing magnesium acetate to magnesium lactate, the same operation as in Production Example 1 was performed to obtain a reconstructed (modified) LDH in which magnesium lactate was intercalated. This is called LDH I-3.
第2部 評価用ゴムシートの作製
ゴムシート;4cm×10cmのサイズに切断し、エタノールで表面を清浄にしたものを使用した
種類;クロロプレンゴムシート(厚さ1mm)
シリコンゴムシート(厚さ0.5mm)
エチレンプロピレンゴムシート(厚さ1mm)
試料;LDH I−1〜3、Mg−Al炭酸型LDH(DHT−6)
Part 2 Preparation of rubber sheet for evaluation Rubber sheet; Type using a sheet cut to a size of 4 cm x 10 cm and cleaned with ethanol; Chloroprene rubber sheet (thickness 1 mm)
Silicon rubber sheet (thickness 0.5mm)
Ethylene propylene rubber sheet (thickness 1mm)
Sample: LDH I-1 to 3, Mg-Al carbonate type LDH (DHT-6)
表1のとおり各試料の水分散体を調製し、これをゴムシートに塗装(両面)・乾燥(80℃)することにより、それぞれ2枚の評価用ゴムシートを作製した。 As shown in Table 1, an aqueous dispersion of each sample was prepared, and two rubber sheets for evaluation were prepared by coating (both sides) and drying (80 ° C.) the rubber sheet.
第3部 ゴムシート上の皮膜の評価
1)皮膜の形成
○;塗装により皮膜が視覚的に確認できる
×;粉体が付いているだけで皮膜を形成していない
2)皮膜の可とう性の評価
○;塗装済みゴムシートを折り曲げても皮膜に割れ(クラック)が入らない
△;折り曲げると割れは入るが、皮膜は剥がれない
×;折り曲げると割れが入り、皮膜が剥がれる
Part 3 Evaluation of the film on the rubber sheet 1) Formation of the film ○: The film can be visually confirmed by painting ×: The film is not formed only by the powder 2) The flexibility of the film Evaluation ○: Even if the painted rubber sheet is folded, no cracks are generated in the film. △: When folded, cracks are formed, but the film does not peel. ×: When folded, cracks enter and the film is peeled off.
第4部 離型性および防着性の確認
評価用ゴムシート2枚を重ね、その上に表面研磨した金属片を置き、1cm2当たり300gの圧力を1分間かけ、金属片とゴムシートの剥がれやすさおよび2枚のゴムシート同士の剥がれやすさを調べた。
Part 4 Confirmation of releasability and adhesion property Two rubber sheets for evaluation were stacked, and a metal piece whose surface was polished was placed thereon, and a pressure of 300 g per 1 cm 2 was applied for 1 minute. The ease of peeling of the rubber sheet and the ease of peeling between the two rubber sheets were examined.
離型性;金属片を持ち上げ、直ちにゴムシートが離れるかで評価した。
○;ゴムシートは全く持ち上がらない
△;ゴムシートも一瞬持ち上がるが、直ちに離れる
×;ゴムシートも持ち上がり、2秒以上離れない
防着性;2枚のゴムシートのうち、上側の端部を持ち上げ、直ちに離れるかで評価した。
○;下側のゴムシートは全く持ち上がらない
△;下側のゴムシートも一瞬持ち上がるが、直ちに離れる
×;下側のゴムシートも持ち上がり、2秒以上離れない
Releasability: Evaluation was made by lifting a metal piece and immediately separating the rubber sheet.
○: The rubber sheet does not lift up at all △: The rubber sheet also lifts up for a moment, but then leaves immediately ×: The rubber sheet also lifts up and prevents adhesion for 2 seconds or more; Of the two rubber sheets, lift the upper end, Evaluation was made by whether to leave immediately.
○: The lower rubber sheet is not lifted at all △: The lower rubber sheet is also lifted for a moment, but is immediately separated ×: The lower rubber sheet is also lifted and is not separated for more than 2 seconds
第5部 紫外線照射による耐水性の変化
表2のとおりLDH I−2の水分散体を調製し、これをゴムシートに塗装(両面)・乾燥(80℃)することにより、合計4枚の評価用ゴムシートを作製した。その内2枚に殺菌ランプ(波長254nm、紫外線出力1.7W、紫外線放射強度19μW/cm2)にて2.5cmの高さから紫外線を2分間照射した後、各ゴムシートの耐水性評価を行った。
Part 5. Change in water resistance due to ultraviolet irradiation As shown in Table 2, an aqueous dispersion of LDH I-2 was prepared, and this was applied to a rubber sheet (both sides) and dried (80 ° C) to obtain a total. Four rubber sheets for evaluation were produced. Two of them were irradiated with ultraviolet rays from a height of 2.5 cm for 2 minutes with a sterilizing lamp (wavelength 254 nm, ultraviolet output 1.7 W, ultraviolet radiation intensity 19 μW / cm 2 ), and then the water resistance of each rubber sheet was evaluated. went.
耐水性評価;ゴムシート表面に蒸留水を0.5ml滴下し、脱脂綿で50回擦った後、表面を視覚的に評価した。
○;変化なし
×;剥がれて脱落する
Evaluation of water resistance: 0.5 ml of distilled water was dropped on the surface of the rubber sheet and rubbed with absorbent cotton 50 times, and then the surface was visually evaluated.
○: No change ×;
Claims (8)
式:Mg1−xAlx(OH)2
(式中、xは0.2〜0.33)を有する複数の基本層の間に、水溶性脂肪族モノカルボン酸マグネシウム塩と層間水がインターカレートされている請求項1の防着剤組成物。 The modified Mg—Al type layered double hydroxide is:
Formula: Mg 1-x Al x (OH) 2
The antiadhesive according to claim 1, wherein a water-soluble aliphatic monocarboxylic acid magnesium salt and intercalation water are intercalated between a plurality of basic layers having the formula (wherein x is 0.2 to 0.33). Composition.
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