200815552 七、 指定代表圖··無 八、 本案若有化學式時，請揭示最能顯示發明特徵的化學式 :無 九、 發明說明： 【發明所屬之技術領域】200815552 VII. Designated representative map·· No. 8. If there is a chemical formula in this case, please disclose the chemical formula that best shows the characteristics of the invention: None Nine, invention description: [Technical field of invention]
I 本發明係有關於提供以雙軸延伸聚丙烯薄膜(BOPP薄膜 )為基材之紙箱封箱用感壓粘著膠帶(稱為B0PP膠帶），所要 求之高保持力（或高内聚力）的乳化型感壓粘著劑。 【先前技術】 傳統乳化類迦著劑無法充分滿足在作為職P膠帶 希望具備高保持力的紙箱封箱用途。為了解決問題而提升了 認為最具影響_聚力。在提㈣聚力的方法上，架橋性單 體的共聚合或架橋劑，例域雜環硫(aziridine)化合物、環 氧化物(epoxy)等的搭配是一般常實施的。但是這種方法只2 提高内聚力，而_力反而降低了，其結果报難同時獲得高 祐著力及内聚力魏化贱壓歸劑。而其他的方法上也嘗 試在壓克力魏膠巾混合了各齡合物等方法。 在日本專利H3-28隨中曾提到混合丙稀酸酿㈣Uc 200815552 ester)變性苯乙烯丁二烯橡膠(SBR)乳化劑之方法；在H3_ m47中提到混合軟化點耽以下的枯著付與劑(taek_方 法；在H3-234781提到混合二烷基二烯丙基鹵化銨(dialkyl diallyl ammonium halide)的方法；在 H2-178381 提到混合聚乙 烯乙一醇本基醚(p〇lyethyiene giyC〇i phenyi ether)的方法及在 H2-202571巾提到混合不同分子量的兩個壓克力乳化型感壓 钻著劑的方法等，但仍然很難同時獲得祕著力及高内聚力 的礼化型感壓枯著齊卜而且也有很難獲得高内聚力的問題以 可耐復原力強之紙箱的反彈性。 【發明内容】 本發明的目的之一為提供適合紙箱封箱之乳化型感壓黏 著劑具有優越_著力、保持力及初期力之平衡 ，其於 BOPP薄膜上塗佈乳化型感壓黏著劑製作成B〇pp膠帶使用 ，疋一具優越的紙箱封箱性之BOPP膠帶。像這樣膠帶的紙 相封相性主要是靠所使㈣乳化型祕黏著_保持力，同 時也必須具有優_崎力及初期力。 的另目的為提供一種適合紙箱封箱之乳化型感 著刻’疋下列形成之單體組成物乳化聚合而獲得的乳化 型感壓枯著_，塗佈於BOPP基材上製成BOPP膠帶時，可 良好地提升保持力與紙箱的封箱性。 200815552 基於上述之目的，本發明係有關—種適合紙箱封箱之 化型感壓黏著劑，除具備紐著力外，更兼具優異保持力。 此乳化型顏轉敝成係包括：⑻絲上具有Μ碳原 子的丙稀_旨單體71·5〜95 5咖_ ; h滅d);⑼具有 3經基可共聚合單體phr; (e) I α，β不餘和羧酸基 (boxyl group )可共聚合單體〇 5〜5咖;⑻可形成同質聚合 體’其玻璃轉移溫度為％以上的可絲合單體純咖;⑻ + (b) + (c) + (d)總量為1〇_。相對於⑻+⑼+⑻+ (d) lOOphr使用(f)非離子界面活性劑，其用量為〇 n力咖; (g)陰離子界面活性劑，其為Μ〜2·恤；必要時可添加 ⑻具架橋基的可共聚合單體，類量為㈣5 _並添加適 里之去_子水、引發劑及緩衝劑，獅—般的乳化具合法製 k而成。本發明之適合封箱之乳化型感壓黏著細固體成分 為30〜70重量％ ’玻璃轉移溫度(Tg)在—2〇。〇〜一贼。 【實施方式】 本發明之適合紙箱封箱之乳化型感壓黏著劑組成成份其 包括： (a)「烷基上具有4〜12碳原子的丙烯酸酯單體」，係指 丙烯酸丁酯、丙烯酸-2乙基己酯、丙烯酸辛酯、丙烯酸癸酯 、丙烯酸異癸酯或丙烯酸月桂脂，其可單獨或是2種以上的 200815552 混合物。在獲得低玻_移溫度且陕_著性上丙婦酸丁 酯、丙烯酸-2乙基己酯較好，其用量範圍為715〜95 5phr。 (b) .「具有含羥基可共聚合單體」，係指丙烯酸羥乙基 醋、曱基丙烯雜乙基g旨、丙烯麵丙基g旨及甲基丙婦酸經 丙基醋的單獨或是2種以上的混合物。特別是較好的單體為 ✓ 丙刘jS文經乙基醋及曱基丙稀酸經乙基醋，其用量範圍含量為 1 〜8 phr。 (c) 「含α，β不飽和竣酸基(carb〇Xyi gr〇Up )可共聚合單體 」，係#曰丙細酸、曱基丙細酸、馬來酸(maleic acid)、富馬酸 (fumaric acid) > S^(itaconic acid) ^ &^^it(crotonic acid) 、單烷基馬來酸(mono alkyl maleic acid)、單烧基富馬酸 (mono alkyl fumaric acid)的單獨或是2種以上的混合物較好 的疋丙細酸及曱基丙烯酸，含量在〇 5phr以下時乳化劑的穩 定性會變差，超過5phr時粘著力會降低，最好的範圍在 1〜4phr 〇 (d) 「可形成同質聚合體，其玻璃轉移溫度為5。〇以上 的可共聚合單體」，係指乙酸乙烯酯、碳素數為1〜4的烧基 甲基丙烯酸脂(alkyl methacrylate)、丙烯腈（acryi〇nitrile)、苯 乙烯(styrene)單獨或是2種以上的混合物，較好的是乙酸乙 烯酯、甲基丙烯酸曱酯、曱基丙烯酸乙酯、甲基丙婦酸丁醋 單獨或是2種以上的混合物，含量3phr以下時無法獲得高内 200815552 聚力的，15phr以上時粘著力會降低，最好的範圍在5〜i2phf 〇 (e)「必要時可添加具架橋基的可共聚合單體」相對於 ⑻+ (b) +⑻+ (d)總量而言，含量為〇〜〇.5 phr，其中含架橋 基的可共聚合單體例如是正—㈣基丙烯醯胺(N_meth咖 acrylamide)，縮水甘油甲基丙稀酸醋(giycidyi methacj^iate)， 乙醯氧基乙基甲基丙烯酸乙酯（acet〇acet〇xy methacrylate)，矽氧化物(Siiane)等。 本發明之乳化型感壓黏著劑，為使在乳化聚合進行時以 達乳化安定性、最終產物具有高粘著力外及優異保持力，可 選用不同類型之界面活性劑之混合組成。其中包括非離子界 面活性劑及陰離子界面活性劑，其含量相對於⑻+ (b) + (c) + (d)總量而言為〇.5-4.5phr。其中： (0「非離子界面活性劑之含量」相對於⑻+ (b) + (c) + (d)總量而言為〇」〜2.〇phr，例如是聚氧乙烯壬基苯基醚、聚 氧乙烯辛基苯基醚、聚乙二醇烧基酚醚、脂肪酸山梨酯或聚 乙^一醇脂肪酸山梨酯。 (g)「陰離子界面活性劑之含量」相對於⑻+ (b) +⑹+ (d)總量而言為〇·4〜2.5phr，例如是十二院基苯續酸鈉、十二 烷基磺酸鈉、磺酸基-十二烷苯基醚二鈉、磺酸基琥珀酸一❿ 十八酯二鈉或聚氧乙烯壬基苯基醚硫酸銨。 200815552 ^ 本發明之乳化型感壓黏著劑組成物可藉由至少一個之引 發劑、緩衝劑及去離子水參與反應。引發劑之使用相對於⑻ + (b) + (c) + (d)總量而言為〇·2〜〇.6phr，例如是過硫酸_、過 硫酸鈉、過硫酸銨、過氧化苯甲醯(benzoyl ρ6ΓΟΧ^)、第三 丁基過氧化氬(t-butyl hydroperoxide)、偶氮雙二異丁腈(ι，2-azobisisobutyronitrile)等。緩衝劑之使用相對於⑻+ (b) +⑹ + (Φ總量而言為〇·2-〇·6ρ1ΐΓ，例如是氫氧化鈉、氳氧化鉀、 ⑩ 碳酸納、石炭酸氫納、石舞酸納、碳酸!弓等。 本發明之乳化型感壓黏著劑在反應槽中進行乳化聚合反 應，將前述⑻、（b)、（c)、（d)及(e)單體，前述(g)及⑻界面活 !·生K物成’亚添如適量之去離子水、引發劑及緩衝劑共 同存在下，加溫受熱_始反應，形成乳膠粒子。反應溫度 為70〜坑’反應時間為5〜1〇小時，即可形成本發明產物。 其產物固體成分為3〇〜7〇%重量，玻璃轉移溫度⑽在〜 零 一50οΓ。 罐壓黏著 200815552 《實施例1》 1、 首先將156g的丙烯酸-2乙基己酯單體[組成⑻]、％的 丙稀酸丁酯單體[組成(a)]、24g丙稀酸經乙基酯單體[組 成(b)]、3g丙稀酸單體[組成(c)]、3g甲基丙稀酸單體[組 成⑹]、12g曱基丙烯酸曱酯單體[組成(d)]及15§甲基丙 〜 烯酸丁酯單體[組成(d)]均勻攪拌製備成A溶液。 2、 另取l〇〇g的去離子水與Ug的聚氧乙烯辛基苯基剛組I The present invention relates to a pressure-sensitive adhesive tape (referred to as a B0PP tape) for providing carton sealing using a biaxially stretched polypropylene film (BOPP film) as a substrate, and a high retention force (or high cohesion) is required. Emulsified pressure sensitive adhesive. [Prior Art] Conventional emulsified carrageenan cannot fully satisfy the purpose of carton sealing in which it is desired to have high retention. In order to solve the problem, the improvement is considered to be the most influential. In the method of (4) cohesion, the copolymerization of a bridging monomer or a bridging agent, such as an aziridine compound, an epoxy, etc., is generally carried out. However, this method only improves the cohesive force, while the _ force is reduced, and the result is difficult to obtain at the same time the high-yield and cohesive force Weihua 贱 pressure returning agent. In other methods, it is also tried to mix various ageing compounds in acrylic rubber towels. In Japanese Patent H3-28, a method of mixing acrylic acid (4) Uc 200815552 ester) styrene butadiene rubber (SBR) emulsifier has been mentioned; in H3_m47, it is mentioned that the mixed softening point is below the dry weight. And taek_method; a method of mixing dialkyl diallyl ammonium halide in H3-234781; mixing polyethylene glycol monoether ether (p〇lyethyiene) in H2-178381 giyC〇i phenyi ether) method and the method of mixing two acrylic emulsified pressure-sensitive drills of different molecular weights in H2-202571, but it is still difficult to obtain secret energy and high cohesion at the same time. The type of pressure is dry and there is a problem that it is difficult to obtain high cohesion to resilience of the carton which is resistant to resilience. One of the objects of the present invention is to provide an emulsified pressure-sensitive adhesive suitable for carton sealing. The agent has superior _ strength, retention and initial force balance. It is coated with emulsified pressure-sensitive adhesive on BOPP film to make B〇pp tape, and it is a superior carton sealing BOPP tape. Tape paper seal The main purpose is to make (4) emulsified type secret adhesion _ retention, but also must have excellent _ saki force and initial force. Another purpose is to provide a emulsified type suitable for carton sealing 刻 疋 疋 疋 疋 疋The emulsified pressure-sensitive adhesive obtained by emulsion polymerization of the composition is dry, and when applied to a BOPP substrate to form a BOPP tape, the holding power and the sealing property of the carton can be favorably improved. 200815552 The present invention is based on the above object. The sensible pressure-sensitive adhesive suitable for carton sealing has excellent retention. In addition, it has excellent retention. The emulsified enamel-forming system includes: (8) propylene having a ruthenium carbon atom on the wire. Monomer 71·5~95 5 _ ; h 灭 d); (9) has 3 via-copolymerizable monomer phr; (e) I α, β and carboxyl group can be copolymerized monomer 〇5~5 coffee; (8) can form a homogeneous polymer's glass transition temperature of more than % of the splicable monomer pure coffee; (8) + (b) + (c) + (d) the total amount is 1 〇 _. (f) + (9) + (8) + (d) lOOphr using (f) a nonionic surfactant, the amount of which is 〇 n 咖 咖; (g) anionic surfactant, which is Μ ~ 2 · shirt; if necessary, can be added (8) A copolymerizable monomer having a bridging group, the amount of which is (4) 5 _ and the addition of a suitable water, an initiator and a buffering agent, and a lion-like emulsification method is legally produced. The emulsified pressure-sensitive adhesive fine solid component suitable for sealing of the present invention is 30 to 70% by weight, and the glass transition temperature (Tg) is -2 Torr. Hey ~ a thief. [Embodiment] The composition of the emulsified pressure-sensitive adhesive suitable for carton sealing of the present invention comprises: (a) "Acrylate monomer having 4 to 12 carbon atoms in the alkyl group", which means butyl acrylate, acrylic acid 2-Ethylhexyl ester, octyl acrylate, decyl acrylate, isodecyl acrylate or lauric acid acrylate, which may be used alone or in combination of two or more of 200815552. In the case of obtaining a low glass-shift temperature, it is preferred to use butyl butyl acrylate and 2-ethylhexyl acrylate in an amount ranging from 715 to 95 5 phr. (b) "having a hydroxyl group-containing copolymerizable monomer" means hydroxyethyl acrylate, decyl propylene heteroethyl ke, propylene propyl propyl group, and methyl propyl acetonate by propyl vinegar alone Or a mixture of two or more. In particular, the preferred monomer is: 3.7 liters of ethyl vinegar and ethyl acetoacetic acid via ethyl vinegar in an amount ranging from 1 to 8 phr. (c) "Alpha-containing β-unsaturated decanoic acid group (carb〇Xyi gr〇Up) copolymerizable monomer", #曰丙细酸, mercaptopropionic acid, maleic acid, rich Fumaric acid > S^(itaconic acid) ^ &^^it(crotonic acid), monoalkyl maleic acid, mono alkyl fumaric acid Separately, or a mixture of two or more kinds of phthalic acid and mercaptoacrylic acid, the stability of the emulsifier may be deteriorated when the content is less than 5 phr, and the adhesion is lowered when the amount is more than 5 phr, and the best range is 1 ~4phr 〇(d) "a homopolymerizable polymer having a glass transition temperature of 5. The copolymerizable monomer above 〇" means vinyl acetate and a methacrylic acid ester having a carbon number of 1 to 4. (alkyl methacrylate), acrylonitrile (acryi〇nitrile), styrene (styrene) alone or a mixture of two or more thereof, preferably vinyl acetate, decyl methacrylate, ethyl methacrylate, methyl propyl Butyl vinegar alone or a mixture of more than 2 kinds, when the content is less than 3 phr, it is impossible to obtain high concentration of 200815552, 15 phr The adhesion will decrease when it is applied. The best range is 5~i2phf 〇(e) "Addable copolymerizable monomer with bridging group if necessary" relative to the total amount of (8) + (b) + (8) + (d) The content is 〇~〇.5 phr, and the copolymerizable monomer containing a bridging group is, for example, N-methacryl acrylamide, glycidic methacj^iate, Acetacetate ethyl methacrylate, bismuth oxide (Siiane), and the like. The emulsified pressure-sensitive adhesive of the present invention may have a mixed composition of different types of surfactants in order to achieve emulsion stability during emulsion polymerization, high adhesion of the final product, and excellent retention. These include nonionic surfactants and anionic surfactants in amounts of from 0.5 to 4.5 phr relative to the total amount of (8) + (b) + (c) + (d). Wherein: (0 "content of nonionic surfactant" is 〇"~2.〇phr, for example, polyoxyethylene nonylphenyl group, relative to the total amount of (8) + (b) + (c) + (d) Ether, polyoxyethylene octyl phenyl ether, polyethylene glycol phenol ether, fatty acid sorbate or polyethyl sorbitol fatty acid sorbate. (g) "content of anionic surfactant" relative to (8) + (b +(6)+ (d) In total, it is 〇·4~2.5phr, for example, 12-base sodium benzoate, sodium dodecyl sulfate, sulfonate-dodecylphenyl ether disodium , sulfosuccinate succinic acid octadecyl ester disodium or polyoxyethylene decyl phenyl ether ammonium sulfate. 200815552 ^ The emulsified pressure sensitive adhesive composition of the present invention can be composed of at least one initiator, buffer and Deionized water participates in the reaction. The use of the initiator is 〇·2~〇.6phr relative to the total amount of (8) + (b) + (c) + (d), for example, persulfate _, sodium persulfate, persulfate Ammonium, benzoyl ruthenium benzoate (benzoyl ρ6ΓΟΧ^), t-butyl hydroperoxide, azo, diazobisisobutyronitrile, etc. The use of a buffer is relative to + (b) +(6) + (In the total amount of Φ, 〇·2-〇·6ρ1ΐΓ, for example, sodium hydroxide, potassium oxyhydroxide, sodium carbonate, sodium hydrogencarbonate, sodium sulphate, carbonic acid! The emulsified pressure-sensitive adhesive of the present invention is subjected to an emulsion polymerization reaction in a reaction tank, and the above-mentioned (8), (b), (c), (d), and (e) monomers are bonded to the above (g) and (8) interfaces. The raw material K is formed into a kind of deionized water, an initiator and a buffering agent in the presence of a proper amount, and is heated and heated to form a latex particle. The reaction temperature is 70~pit, and the reaction time is 5 to 1 hour. The product of the present invention can be formed. The solid content of the product is 3〇~7〇% by weight, and the glass transition temperature (10) is in the range of 〜50-50Γ. The can pressure bonding 200815552 "Example 1" 1. First, 156g of 2-ethyl acrylate Hexyl ester monomer [composition (8)], % butyl acrylate monomer [composition (a)], 24 g of acrylic acid via ethyl ester monomer [composition (b)], 3 g of acrylic acid monomer [composition (c)], 3 g of methyl acrylate monomer [composition (6)], 12 g of decyl decyl acrylate monomer [composition (d)] and 15 § methyl propyl ethenoate monomer [composition (d) Uniform stirring preparation Into A solution. 2. Another l〇〇g deionized water and Ug polyoxyethylene octyl phenyl group
• 成⑼及6邶十二烷基磺酸鈉[組成(g)]均勻攪拌製備成B 溶液。 3、 將A溶液到入b溶液持續攪拌製備成預乳化。溶液。 4、 另取88·5的去離子水製備成D溶液。 - 5另取43g的去離子水、ι·5碳酸氫鈉及185g的過硫酸钟 均勻攪拌製備成E溶液。 另取15g的去離子水及〇 ig的過硫酸钟均勻擾摔製備成 籲 F溶液。 7、將D騎倒人乳化聚合設備，其包括：授掉器、溫度計 、加熱器、迴流冷凝管、五頸及—公升圓底瓶中。加熱 至80-82 C B夺’再將F溶液到入轉1〇_15分鐘。然後c 溶液分別在240分鐘喂入完畢。然後將溫度升至85_ 87 C將F溶液1〇分鐘喂入完畢並維持9〇分鐘後冷卻至 室溫。所得乳化型感壓黏著劑之固體成份為 55.0% 〇 將 10 200815552 其塗佈於BOPP薄膜後，其物性測試結果參照下述表二 Ο 《實施例2》 1、 首先將156g的丙烯酸-2乙基己酯單體[組成(a)]、87g的 丙烯酸丁酯單體[組成⑻]、12g丙烯酸羥乙基酯單體[組 成(b)]、3g丙稀酸單體[組成⑹]、3g曱基丙烯酸單體[組 成⑻]、12g曱基丙烯酸曱酯單體[組成(d)]、15g曱基丙 烯酸丁酯單體[組成(d)]及12g乙酸乙烯醋單體[組成⑹] 均勻攪:摔製備成A溶液。 2、 另取l〇〇g的去離子水與Ug的聚乙二醇烷基酚_[組成 (f)]及6.0g磺酸基-十二烷苯基醚二鈉[組成均勻攪拌 製備成B溶液。 3、 將A溶液到入b溶液持續攪拌製備成預乳化c溶液。 4、 另取88.5的去離子水製備成d溶液。 5、 另取43g的去離子水、15碳酸氫鈉及h85g的過硫酸钟 均勻擾拌製備成E溶液。 6、 另取15g的去離子水及〇 lg的過硫酸鉀均勻攪拌製備成 F溶液。• Sodium (9) and 6-dodecylsulfonate [composition (g)] were uniformly stirred to prepare a B solution. 3. Pre-emulsification is prepared by continuously stirring the solution A into the solution b. Solution. 4. Another 88.5 deionized water was prepared to prepare a D solution. - 5 Another 43 g of deionized water, 1⁄5 sodium hydrogencarbonate and 185 g of persulfate clock were uniformly stirred to prepare an E solution. Another 15 g of deionized water and 〇 ig of persulfate clock were evenly disturbed to prepare a F solution. 7. D rides the human emulsion polymerization equipment, which includes: a transfer device, a thermometer, a heater, a reflux condenser, a five-neck and a liter round bottom bottle. Heat to 80-82 C B and then transfer the F solution to 1 〇 for 15 minutes. Then the c solution was fed in 240 minutes. The temperature was then raised to 85-87 C and the F solution was fed for 1 minute and maintained for 9 minutes and then cooled to room temperature. The solid content of the obtained emulsified pressure-sensitive adhesive is 55.0%. After applying 10200815552 to BOPP film, the physical property test results refer to the following Table 2. "Example 2" 1. First, 156g of acrylic acid-2B Hexyl hexyl ester monomer [composition (a)], 87 g of butyl acrylate monomer [composition (8)], 12 g of hydroxyethyl acrylate monomer [composition (b)], 3 g of acrylic acid monomer [composition (6)], 3 g of mercaptoacrylic acid monomer [composition (8)], 12 g of decyl decyl acrylate monomer [composition (d)], 15 g of butyl methacrylate monomer [composition (d)], and 12 g of vinyl acetate monomer [composition (6) ] Evenly stir: drop into a solution A. 2. Another l〇〇g of deionized water and Ug of polyethylene glycol alkyl phenol _ [composition (f)] and 6.0 g of sulfonic acid-dodecyl phenyl ether disodium [formally stirred to prepare B solution. 3. Prepare the pre-emulsified c solution by continuously stirring the solution A into the solution b. 4. Another 88.5 deionized water was prepared to prepare a d solution. 5. Another 43 g of deionized water, 15 sodium bicarbonate and h85 g of persulfate clock were uniformly mixed to prepare an E solution. 6. Another 15 g of deionized water and lg lg of potassium persulfate were uniformly stirred to prepare an F solution.
7將D冷/夜倒入乳化聚合設備，其包括：攪拌器、溫度計 、加熱☆'、迴流冷凝管、五頸及—公升圓底瓶中。加熱 至8〇_82ΐ：時，再將F溶液到入維持10-15分鐘。然後C 11 200815552 >谷液分別在240分鐘喂入完畢。然後將溫度升至85_ 87 C將F溶液10分鐘喂入完畢並維持9〇分鐘後冷卻至 室溫。所得乳化型感壓黏著劑之固體成份為55·〇%。將 其塗佈於ΒΟΡΡ薄膜後，其物性測試結果參照下述表二 〇 《比較實施例1》 1、 首先將156g的丙烯酸-2乙基己酯單體[組成⑻]、 的丙烯酸丁酯單體[組成⑻]、12g丙烯酸羥乙基酯單體[ 組成(b)]、12g丙烯酸單體[組成⑷]及〇 6g乙醯氧基乙基 曱基丙烯酸乙酯[組成(e)]均勻攪拌製備成A溶液。 2、 另取100g的去離子水與Ug㈣氧乙稀壬基苯基醚[組 成(0]及6.0g聚氧乙烯壬基苯基_硫酸銨[組成(g)]均勻 攪拌製備成B溶液。 3、 將A溶溶液持續攪拌製備成雜紅溶液。 4、 另取88.5的去離子水製備成1)溶液。 5、 另取43g的去離子水、15碳酸氫鈉及18化的過硫酸钟 均勻攪拌製備成E溶液。 6另取15g的去離子水及〇 lg的過硫酸钟均句擾摔製備成 F溶液。 7、將D溶液倒人乳化聚合設備，其包括：授摔器、溫度計 、加熱器、迴流冷凝管、五頸及—公升圓底瓶中。加熱 12 200815552 至80-82°C時，再將F溶液到入維持1(M5分鐘。然後c 溶液分別在24G分鐘喂入完畢。然後將溫度升至似rc 將F溶液10分鐘喂入完畢並維持9〇分鐘後冷卻至室溫 。所得乳化型感壓黏著劑之固體成份為55麗。將其塗佈 於BOPP薄膜後，其物性測試結果參照下述表二。 《比較實施例2》 1、 首先將156g的丙烯酸_2乙基己酿單體[組成⑼]、12% 的丙烯酸丁酯單體[組成⑻]、12g丙烯酸羥乙基酯單體[ 組成(b)]、12g丙烯酸單體[組成卜)]及〇 6g正羥甲基丙 烯醯胺[組成(e)]均勻攪拌製備成a溶液。 2、 另取100g的去離子水與18g的聚氧乙烯壬基苯基醚[組 成⑼及6.0g聚氧乙烯壬基苯基醚硫酸銨[組成(g)]均勻 攪拌製備成B溶液。 3、 將A溶液到入B溶液持續攪拌製備成預乳化c溶液。 4、 另取88·5的去離子水製備成〇溶液。 5、 另取43g的去離子水、15碳酸氳鈉及185g的過硫酸鉀 均勻攪拌製備成E溶液。 6、 另取15g的去離子水及〇 lg的過硫酸鉀均勻攪拌製備成 F溶液。 7、 將D溶液倒入乳化聚合設備，其包括攪拌器、溫度計 、加熱器、迴流冷凝管、五頸及一公升圓底瓶中。加熱 13 200815552 至80魏時，再將F溶液到入維持㈣分鐘。然後c 溶液分別在分鐘喂人轉。贿躲度升至％机 將F /合液1〇分|里喂入完畢並維持如分鐘後冷卻至室溫 。所得乳化壓輯敗固體成份為5通。將其塗 佈於BOPP薄膜後’其物性測試結果參照下述表二。 表-、本發明實施例卜2、比較實施例卜2使用之單體組 成(a)〜(e)比較表如下所示。7 P cold/night into the emulsion polymerization equipment, which includes: agitator, thermometer, heating ☆', reflux condenser, five neck and - liter round bottom bottle. When heating to 8 〇 _82 ΐ:, the F solution is maintained for 10-15 minutes. Then C 11 200815552 > trough was fed in 240 minutes. The temperature was then raised to 85-87 C and the F solution was fed for 10 minutes and maintained for 9 minutes and then cooled to room temperature. The obtained emulsified pressure-sensitive adhesive had a solid content of 55% by weight. After coating it on a ruthenium film, the physical property test results thereof are as follows: Comparative Example 1 1. First, 156 g of -2-ethylhexyl acrylate monomer [composition (8)], butyl acrylate alone Body [composition (8)], 12 g of hydroxyethyl acrylate monomer [composition (b)], 12 g of acrylic monomer [composition (4)] and 〇 6 g of ethyl ethoxyethyl methacrylate [composition (e)] uniform Stir to prepare the A solution. 2. Another 100 g of deionized water and Ug (tetra) oxyethylene phenyl phenyl ether [composition (0] and 6.0 g of polyoxyethylene nonylphenyl sulfonate [composition (g)] were uniformly stirred to prepare a B solution. 3. Prepare the red solution by continuously stirring the solution A. 4. Prepare 1) solution by taking 88.5 deionized water. 5. Another 43 g of deionized water, 15 sodium bicarbonate and 18 persulfate clocks were uniformly stirred to prepare an E solution. 6 Another 15g of deionized water and lg lg of persulfate bells were used to prepare the F solution. 7. The D solution is poured into an emulsion polymerization equipment, which includes: a drop detector, a thermometer, a heater, a reflux condenser, a five-neck and a liter round bottom bottle. When heating 12 200815552 to 80-82 ° C, the F solution is added to maintain 1 (M5 minutes. Then the c solution is fed in 24G minutes respectively. Then the temperature is raised to rc and the F solution is fed for 10 minutes. After maintaining for 9 minutes, it was cooled to room temperature. The obtained emulsified pressure-sensitive adhesive had a solid content of 55 Å. After coating it on a BOPP film, the physical property test results are shown in Table 2 below. Comparative Example 2 First, 156 g of 2-ethylhexyl acrylate monomer [composition (9)], 12% butyl acrylate monomer [composition (8)], 12 g of hydroxyethyl acrylate monomer [composition (b)], 12 g of acrylic acid The body [composition] and 〇6g of n-hydroxymethylpropenylamine [composition (e)] were uniformly stirred to prepare a solution. 2. Another 100 g of deionized water and 18 g of polyoxyethylene nonylphenyl ether [composition (9) and 6.0 g of polyoxyethylene nonylphenyl ether sulfate [composition (g)] were uniformly stirred to prepare a B solution. 3. Prepare the pre-emulsified c solution by continuously stirring the solution A into the solution B. 4. Another 88.5 deionized water is used to prepare a bismuth solution. 5. Another 43 g of deionized water, 15 sodium strontium carbonate and 185 g of potassium persulfate were uniformly stirred to prepare an E solution. 6. Another 15 g of deionized water and lg lg of potassium persulfate were uniformly stirred to prepare an F solution. 7. Pour D solution into an emulsion polymerization unit that includes a stirrer, thermometer, heater, reflux condenser, five neck and one liter round bottom bottle. Heating 13 200815552 to 80 Wei, then the F solution is maintained for (four) minutes. Then the c solution was fed in minutes. The bribes are raised to the % machine. F / 1 liquid is added to the machine and the feed is completed and maintained as room temperature and then cooled to room temperature. The obtained emulsified pressure-collecting solid component is 5-pass. After coating it on a BOPP film, the physical property test results are shown in Table 2 below. Table - Inventive Example 2, Comparative Example 2 The monomer compositions used in (a) to (e) are shown below.
〇：有添加；X無添加 《測試樣品之製作》 使用BOPP /專膜厚度為25胖，塗佈本發明實施例1、2 14 200815552 、比較實施例1 '2所得之乳化型感壓粘著劑，塗佈厚度為 20μηι，以下列測試方法進行紙箱封箱試驗(性能編號丨）、鋼 板枯著力（性能編號2)、紙板破壞面積··（性能編號3)及紙板 保持力（性能編號4)，其物性測試結果參照下述表二。 《測試方法》 紙箱封箱試驗:(性能編號1)〇: added; X no added "production of test sample" using BOPP / film thickness of 25 fat, coating the inventive example 1, 2 14 200815552, comparative example 1 '2 obtained by emulsion pressure adhesive The coating was applied at a thickness of 20 μm, and the carton sealing test (performance number 丨), steel plate dryness (performance number 2), cardboard damage area (performance number 3), and paperboard retention (performance number 4) were tested by the following test methods. ), the physical property test results refer to Table 2 below. "Test Method" Carton Sealing Test: (Performance No. 1)
製作5cmx40Cm的膠帶在3〇cmx3〇cmx3〇cm瓦擇紙製作 而成的雙層紙箱兩邊_式的密合線上貼上膠帶封箱， 谬帶兩邊料-，放置於23t>6_龍度_、 -20。〇40% RH 一個星期，每轉 ㈣口，卿魏_嶋目，數目=_ 箱封箱試驗效果愈差。 2、鋼板粘著力··（性能編號2) 依照ASTM D4000標準。Make 5cmx40Cm tape and put it on the double-sided carton made of 3〇cmx3〇cmx3〇cm tile paper. Apply the tape to the tight line on both sides of the _ type, and put it on both sides. Place it on 23t>6_龙度_ , -20. 〇40% RH One week, every turn (four) mouth, Qing Wei _ eye, number = _ The result of the box sealing test is worse. 2. Steel plate adhesion · (performance number 2) According to ASTM D4000 standard.
紙板破壞面積：（性能編號3) 製作、5cmxl5cm的膠帶，貝占於標準紙板_!次，使用 劃格法’計算紙板被撕破面積(％)。 紙板保持力：（性能編號4) •5cm，貼於 ^照美國PSTC-7標準，樣品尺寸為25cm><i 標準紙板，荷重lkg，紀騎科之時間。 4、 200815552 ^施例卜2、比較實施例1及2之物性比較表Cardboard damage area: (Performance No. 3) Manufactured, 5cmxl5cm tape, shelled on standard cardboard _! times, using the cross-cut method' to calculate the torn area (%) of the cardboard. Cardboard retention: (Performance No. 4) • 5cm, attached to the US PSTC-7 standard, sample size is 25cm><i standard cardboard, load lkg, Jiqike time. 4, 200815552 ^Example 2, comparison of physical properties of Comparative Examples 1 and 2
性倉丨 -----1 實施例1 實施例2 比較實施例1 比較實施例2 1 紙箱封箱試驗 (紙箱翹開個數） 23〇Cx65%RH 0 0 3 1 -20〇Cx40%RH 0 0 5 2 2 鋼板粘著力(kg/in) 0.72 0.75 0.50 0.43 3 紙板破壞面積(％) 96 98 85 70 4 紙板保持力(分鐘) 1000 1050 100 1 CA 13U 上膠條件:BOPP薄膜厚度25_;上膠厚度2〇师。 由表二可知，在紙箱封箱試驗結果(性能編號1)，實施 例1及2具有優異的紙箱封箱試驗，在環境為23。〇65%四 及-20°Cx40%RH日夺，其數字均為〇，其代表紙箱皆未麵開 。然而，比較實施例1及2在環境為23°Cx65%RH時，為分 別有3個及1個紙箱翹開，在環境為一2〇c^x4〇%rh時，分 別有5個及2個紙箱翹開。 在鋼板枯著力（性能編號2)及紙箱板破壞面積(性能編號 3)試驗結果，實施例1及2也較比較實施例1及比較實施例 2優異。貫施例1及2之鋼板粘著力分為〇72 kg/in及 〇.75kg/m’而比較實施例1及比較實施例2分別僅有〇·5〇 kg/in 及 0.43 kg/in 〇 在紙箱板破壞面積(性能編號3)試驗結果顯示，實施例1 16 200815552 及2之紙箱板破壞面積分為96%及98%，而比較實施例1及 比較實施例2分別僅有85%及70%。 在紙板保持力（性能編號4)試驗結果中，實施例1及2 分別高達1000及1〇5〇分鐘，然而比較實施例1及比較實施 例2僅有1〇〇及150分鐘。 由此可見本明之適合紙箱封箱之乳化型感壓黏著劑具有 下例優點··紙箱封箱試驗(性能編號υ、鋼板粘著力（性能編 號2)、紙箱板破壞面積(性能編號3)及紙板保持力(性能編號 4)。 ~ m貫施例伽轉例說明本發明的目的、技術内容 特點及功效，並_來舰本發。 【圖式簡單說明】 鲁 【主要元件符號說明】Sexual Warehouse -----1 Example 1 Example 2 Comparative Example 1 Comparative Example 2 1 Carton sealing test (number of carton cockings) 23〇Cx65%RH 0 0 3 1 -20〇Cx40%RH 0 0 5 2 2 Adhesion of steel plate (kg/in) 0.72 0.75 0.50 0.43 3 Damage area of cardboard (%) 96 98 85 70 4 Paperboard retention (minutes) 1000 1050 100 1 CA 13U Gluing conditions: BOPP film thickness 25_; Glue thickness 2 〇 division. As can be seen from Table 2, in the carton sealing test results (performance number 1), Examples 1 and 2 had an excellent carton sealing test, and the environment was 23. 〇 65% 4 and -20 ° C x 40% RH, the figures are all 〇, which means that the carton is not open. However, in Comparative Examples 1 and 2, when the environment is 23 ° C x 65% RH, there are 3 and 1 cartons respectively, and when the environment is 2 〇 c ^ x 4 〇 % rh, there are 5 and 2 respectively. The cardboard boxes are tilted open. In the test results of the steel sheet dryness (performance number 2) and the carton board failure area (performance number 3), Examples 1 and 2 were also superior to Comparative Example 1 and Comparative Example 2. The adhesion of the steel sheets of Examples 1 and 2 was 〇72 kg/in and 〇.75 kg/m', and Comparative Example 1 and Comparative Example 2 were only 〇·5〇kg/in and 0.43 kg/in, respectively. The test results of the carton board failure area (performance number 3) show that the destruction area of the carton board of the example 1 16 200815552 and 2 is 96% and 98%, while the comparative example 1 and the comparative example 2 are only 85% and 70%. In the results of the paperboard retention (performance number 4) test, Examples 1 and 2 were as high as 1000 and 1.5 minutes, respectively, whereas Comparative Example 1 and Comparative Example 2 were only 1 and 150 minutes. It can be seen that the emulsified pressure-sensitive adhesive suitable for carton sealing has the following advantages: · Carton sealing test (performance number υ, steel plate adhesion (performance number 2), carton board failure area (performance number 3) and Cardboard retention (performance number 4). ~ m example of gamma conversion examples to illustrate the purpose, technical content and efficacy of the present invention, and _ to ship the ship. [Simple diagram] Lu [main symbol description]