TW201020281A - Fog-proof coating composition, fog-proof film and products thereof - Google Patents
Fog-proof coating composition, fog-proof film and products thereof Download PDFInfo
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- TW201020281A TW201020281A TW97146398A TW97146398A TW201020281A TW 201020281 A TW201020281 A TW 201020281A TW 97146398 A TW97146398 A TW 97146398A TW 97146398 A TW97146398 A TW 97146398A TW 201020281 A TW201020281 A TW 201020281A
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201020281 六、發明說明： 【發明所屬之技術領域】 本發明係關於一種防霧塗層組合物、防霧薄膜和製 尤扎種特別適用於尚溫高濕環境下的防霧塗層組合 5物、包含由該組合物製成的塗層的防霧薄膜和包含該防霧 薄膜的製品’例如醫療手術面罩。201020281 VI. Description of the Invention: [Technical Field] The present invention relates to an anti-fog coating composition, an anti-fog film and an anti-fog coating composition which are particularly suitable for use in a warm and humid environment. An antifogging film comprising a coating made of the composition and an article comprising the antifogging film, such as a medical surgical mask.
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【先前技術】 塑膠或者無機透明材料是我們日常生活中經常用到 的’這_料的-個共同問題是結霧後其透明性會受到很 大的影響。例如，在手術過程中，如果醫生用的手術面罩 ^結霧現象嚴重’會對手術造成不可估量的後果。爲了解 決這個問題，各種防霧塗層應運而生。 塗層的防霧性會隨著溫度和濕度的上升而下降，尤1 塗層的防霧性影響非常大。而通常這類防霧産品 ::要求一定的保質期’如果儲存或者運輸過程中有大量 的南溫，産品很可能失效’例如在％攝氏度嶋 不到12個小時就會失去防霧性能。測試 ==如血_試試紙，孕檢試紙尿 要具有穩定的親水表φ。 守也需 四此[Prior Art] Plastic or inorganic transparent materials are often used in our daily lives. A common problem is that transparency will be greatly affected after fogging. For example, in the course of surgery, if the surgical mask used by the doctor is severely fogged, it will have immeasurable consequences for the operation. In order to solve this problem, various anti-fog coatings have emerged. The anti-fog property of the coating will decrease with the increase of temperature and humidity, and the anti-fog property of the coating is very large. Usually, such anti-fog products require a certain shelf life. If there is a large amount of south temperature during storage or transportation, the product is likely to fail. For example, in % Celsius, the anti-fog performance will be lost in less than 12 hours. Test == If blood _ test paper, pregnancy test paper urine should have a stable hydrophilic table φ. Shou also needs four
w仍需要開發一種能夠用於在高溫高 下長時間保純切雜能賴霧H 濕環境 【發明内容】 20 201020281 本發明的一個目的是提供 境下的防霧塗層組合物，尤1是=料用於高溫高濕環 5 ❹ 10 15There is still a need to develop a wet environment capable of maintaining high purity at high temperatures for a long period of time. [Invention] 20 201020281 An object of the present invention is to provide an anti-fog coating composition under the environment, in particular = material for high temperature and high humidity ring 5 ❹ 10 15
尤其疋耠供一種特別適用於高溫 "餘境下既能防霧又能防黏的防霧塗層組合物。 的塗一個目的是提供一種包含由該組合物製成 的塗層的親水防霧薄膜。 發㈣再自目的是提供—種包含該穩㈣親水防 ㈣膜的製品’例如面罩、眼鏡、廣告箱、展示櫥窗、攝 像鏡頭、測試器材。 在高溫高濕的環境下’聚乙稀醇塗層很容易老化結 霧我們的實驗結果表明在5〇攝氏度，9〇%的相對濕度下， 聚乙烯醇塗層在ΡΕΤ上的老化防霧時間不超過2個小時。本 發明的發明人發現，利用聚乙烯醇作爲主要組分並加入特 定量的陰離子表面活性劑得到的塗層組合物能夠提供一種 性能優異的防霧塗層，該防霧塗層不僅能夠耐高溫高濕老 化’而且具有改善的抗黏能力。將本發明的塗層組合物塗 布在基材上形成的薄膜可以成捲或堆疊放置而沒有黏連現 象。 由此，本發明的第一個方面，提供了一種防霧塗層組 20 合物，其包含： 至少一種親水性聚合物； 按聚合物重量爲100重量％計，0.5重量％到25重量。/〇的 至少一種陰離子表面活性劑； 按聚合物重量爲100重量％計，0重量％到60重量％的無 25 毒的或低毒的無機氧化物顆粒；和 4 201020281 5 ❹ 10 15 ❹ 20 其中所述的聚合物選自纖維素、聚乙烯基β比咯烷酮、 聚丙烯酸、聚丙烯醯胺、聚乙烯醇中的至少一種。 本發明的另一個方面，提供了一種親水防霧薄膜，其 包含基材和位於該基材至少一面的至少一部分上並由該組 合物製成的塗層。 本發明的再一個方面，提供了一種包含本發明的穩定 的親水防霧薄膜的製品’例如面罩 '眼鏡、廣告箱、展示 櫥窗、攝像鏡頭、測試器材。 【實施方式】 本發明中，除非另外指出，否則術語“高溫，，是指攝氏 40度以上，術語“高濕”是指8〇%以上的濕度。 除非另外指出’術語“奈米級，，是指平均粒徑爲15〇奈 米以下。 除非另外指出’術語“表面活性劑，，指的是同一分子上 同時具有親水（極性）和憎波r w 和僧水（非極性）基團的能夠降低 =溶液表面張力的分子。有用的表面活性劑可能包括美 :專利_侧3 (Scholz等人，該專利引入本文作爲參 考）中提到的那些。 含 本發明的一個方面提供了 _ „ ^ ^ 刀w捉伢了 —種防霧塗層組合物，其包 至少一種親水性聚合物； 按聚合物重量爲1〇〇重詈。/ 4 篁A计，0.5重量％到25重量％ 5 201020281 的至少一種陰離子表面活性劑； 按聚合物重量爲1〇〇重量％計，〇重量％到6〇重量％的 無毒的或低毒的無機氧化物顆粒；和 溶劑； 5 其中所述的聚合物選自纖維素、聚乙烯基"比咯烷嗣、 聚丙烯酸、聚丙烯酰胺、聚乙烯醇中的至少一種。 根據某些優選的實施方案，其中所述的聚合物的分子 量爲 9000-150000。 根據較佳的實施方案，其中所述的親水性聚合物爲聚 10 乙烯醇。 聚乙烯醇是一種常見的高分子，由於其側鏈上富集的 經基而使其具有良好的親水防霧性能。但是，其防霧性能 會隨著溫度和濕度的升高而急劇下降。使用聚乙烯醇作爲 防霧塗層的另外一個問題是發黏，尤其在高溫高濕條件 15下，聚乙烯醇塗層之間相互接觸會產生黏連，從而導致塗 層的破壞。但是，本發明人發現，採用特定的陰離子表面 活性劑與聚乙稀醇組合，能夠同時有效地避免其在高溫高 濕條件下的防霧性能下降問題和發黏問題。 有用的陰離子表面活性劑包括，但不限於那些具有以 20 下結構的分子（1 )至少一個憎水結構部分，例如〇6到C2〇 左右的烧基’烧基芳基和/或鏈烯基；（2)至少一個阶離 子基團，例如硫酸根、磺酸根、磷酸根、聚氧乙烯硫酸根、 聚氧乙烯續酸根、聚氧乙烯麟酸根等；和/或者（3)此類 陰離子基團的鹽，其中所述鹽包括鹼金屬鹽、銨鹽、叔氨 6 201020281 • 基鹽等。適用的陰離子表面活性劑的已經商品化的代表性 例子包括：十二烷基苯磺酸鈉（例如以商品名SIPONATE DS-10 購自 Rhone-Poulenc，Inc.，Cranberry, N.J.)、十二 烷基硫酸鈉（例如以商品名TEXAPON L_100購自Henkel 5 Inc” Wilmington，Del·,或以商品名 POLYSTEP B-3 購自 Stepan Chemical Co, Northfield, 111.)、十二烧基謎硫酸納 (例如以商品名 POLYSTEP B-12 購自 Stepan Chemical Co., Northfield, 111.)、十二烧基硫酸錄（例如以商品名 參 STANDAPOL A 構自 Henkel Inc., Wilmington，Del. )、1，4_ 10 二（2-乙基己基）-磺酸鈉（例如以商品名GR-5M購自陶氏中 國有限公司）等。 加入另外一種不具有防霧性能的潤濕劑可以提高塗 層的均勻性。有用的潤濕劑包括聚氧乙烯化烷基醇（例如 "Brij™ 30，"和"BrijTM 35，"可購自 ICI Americas，Inc·; 15 "TergitolTM TMN-6TM Specialty Surfactant,” 可購自 Union Carbide Chemical and Plastics Co.)、聚氧乙稀化烧基紛（例 ⑩ 如，"Triton™ X-100” ，可購自 Union Carbide Chemical andIn particular, it is provided with an anti-fog coating composition which is particularly suitable for high temperature "anti-fog and anti-adhesion. One purpose of the coating is to provide a hydrophilic antifogging film comprising a coating made from the composition. The hair (4) is also intended to provide a product comprising the stable (four) hydrophilic (four) film, such as a mask, glasses, an advertising box, a display window, a camera lens, and a test device. In high temperature and high humidity environment, the polyethylene coating is easy to aging and fogging. Our experimental results show that the aging anti-fog time of the polyvinyl alcohol coating on the crucible at 5 ° C, 9 〇 % relative humidity No more than 2 hours. The inventors of the present invention have found that a coating composition obtained by using polyvinyl alcohol as a main component and adding a specific amount of an anionic surfactant can provide an antifogging coating excellent in performance, and the antifogging coating can not only withstand high temperature High humidity aging 'and improved resistance to sticking. The film formed by coating the coating composition of the present invention on a substrate can be placed in a roll or in a stack without sticking. Thus, in a first aspect of the invention, there is provided an anti-fog coating composition comprising: at least one hydrophilic polymer; from 0.5% by weight to 25 parts by weight based on 100% by weight of the polymer. At least one anionic surfactant of hydrazine; from 0% by weight to 60% by weight, based on the weight of the polymer, of non-25 toxic or low toxic inorganic oxide particles; and 4 201020281 5 ❹ 10 15 ❹ 20 The polymer described therein is at least one selected from the group consisting of cellulose, polyvinyl β-pyrrolidone, polyacrylic acid, polyacrylamide, and polyvinyl alcohol. In another aspect of the invention, a hydrophilic antifogging film comprising a substrate and a coating on at least a portion of at least one side of the substrate and made of the composition is provided. In still another aspect of the invention, there is provided an article comprising a stable hydrophilic antifogging film of the invention, such as a mask, an eyeglass, an advertising case, a display window, a camera lens, a test device. [Embodiment] In the present invention, unless otherwise indicated, the term "high temperature" means 40 degrees Celsius or more, and the term "high humidity" means humidity above 8 %. Unless otherwise indicated by the term "nano", It means that the average particle size is 15 〇 or less. Unless otherwise indicated, the term "surfactant" refers to a molecule on the same molecule that has both hydrophilic (polar) and chopped rw and hydrophobic (non-polar) groups capable of reducing the surface tension of the solution. Useful surface activity Agents may include those mentioned in U.S. Patent No. 3 (Scholz et al., the disclosure of which is incorporated herein by reference). A composition comprising at least one hydrophilic polymer; 1 〇〇 by weight of the polymer. / 4 篁A, 0.5% by weight to 25% by weight of 5 201020281 of at least one anionic surfactant; 9% by weight of the polymer, 〇% by weight to 6% by weight of non-toxic or low-toxic Inorganic oxide particles; and a solvent; wherein the polymer is at least one selected from the group consisting of cellulose, polyvinyl, pyrrolidine, polyacrylic acid, polyacrylamide, and polyvinyl alcohol. According to certain preferred embodiments, the polymer has a molecular weight of from 9000 to 150,000. According to a preferred embodiment, the hydrophilic polymer is poly 10 vinyl alcohol. Polyvinyl alcohol is a common polymer which has good hydrophilic anti-fog properties due to its enriched meso group on its side chain. However, its anti-fog performance drops sharply with increasing temperature and humidity. Another problem with the use of polyvinyl alcohol as an anti-fog coating is that it is tacky, especially under high temperature and high humidity conditions, and the contact of the polyvinyl alcohol coatings with each other causes adhesion, which causes damage to the coating. However, the inventors have found that the combination of a specific anionic surfactant and polyethylene glycol can effectively avoid the problem of the antifogging property and the stickiness problem under high temperature and high humidity conditions at the same time. Useful anionic surfactants include, but are not limited to, those having at least one hydrophobic structure of the molecule (1) having a structure of 20, such as a decyl aryl group and/or an alkenyl group of from about 6 to about C2. (2) at least one ionic group such as sulfate, sulfonate, phosphate, polyoxyethylene sulfate, polyoxyethylene sulphate, polyoxyethylene sulphate, etc.; and/or (3) such anionic group a salt of the group, wherein the salt includes an alkali metal salt, an ammonium salt, a tertiary ammonia 6 201020281 • a base salt, and the like. Representative examples of suitable anionic surfactants that have been commercialized include sodium dodecylbenzene sulfonate (e.g., from Rhone-Poulenc, Inc., Cranberry, NJ under the trade name SIPONATE DS-10), dodecane Sodium sulfate (for example, available from Henkel 5 Inc under the trade name TEXAPON L_100, Wilmington, Del., or from Stepan Chemical Co, Northfield, 111.) under the trade name POLYSTEP B-3, Available under the trade name POLYSTEP B-12 from Stepan Chemical Co., Northfield, 111.), 12-alkyl sulphate (for example, under the trade name STANDAPOL A from Henkel Inc., Wilmington, Del.), 1, 4-10 Sodium bis(2-ethylhexyl)-sulfonate (for example, commercially available from Dow China Ltd. under the trade name GR-5M), etc. Adding another wetting agent that does not have antifogging properties can improve the uniformity of the coating. Useful wetting agents include polyoxyethylated alkyl alcohols (e.g. "BrijTM 30," and "BrijTM 35," available from ICI Americas, Inc.; 15 "TergitolTM TMN-6TM Specialty Surfactant, Can be purchased from Union Carbide Chemical and Plas Tics Co.), polyoxyethylene smelting base (example 10, for example, "TritonTM X-100", available from Union Carbide Chemical and
Plastics Co. ； "Iconol™ NP_70"，可購自 BASF Corp.)和 聚乙二醇/聚丙二醇嵌段共聚物（均可以"TetronicTM 1502 20 Block Copolymer Surfactant," "Tetronic™ 908 Block Copolymer Surfactant"和 "PluronicTM F38 Block Copolymer Surfactant，"購自 BASF，Corp.)。當然，任何加 入的潤濕劑的加入量必須以不破壞塗層的防霧性能爲準。 根據二氧化矽奈米級顆粒的用量，基於塗層組合物的總重 25 量，潤濕劑的用量通常低於約0.1重量％，較佳爲約0.003- 201020281 0.05重量％。漂洗或將塗層製品浸泡在水中可以除去過量 的表面活性劑或潤濕劑。 5 參 10 15 參 根據某些優選的實施方案，適用於本發明的陰離子表 面活性劑包括’但不限於：羧酸鹽類、硫酸鹽類、鱗酸鹽 類（包括單、雙酯鹽）、含氟陰離子表面活性劑以及續酸 類或磺酸鹽類表面活性劑。其中較佳為磺酸類和磺酸鹽類 陰離子表面活性劑。其中更佳為仲烷基磺酸鹽，如仲烷基 磺酸鈉、烷基苯磺酸，如十二烷基苯磺酸、烷基苯磺酸鹽， 如十二烷基苯績酸鈉、和琥珀酸酯磺酸鹽，如丨，4-二（2_ 乙基己基）-續酸納。 根據某些優選的實施方案，本發明採用十二烷基苯磺 酸和/或十二烷基苯磺酸鈉作爲陰離子表面活性劑。這兩種 表面活性劑在提局聚乙烯醇塗層的防黏效果方面尤其優 異。雖然不願受理論的束缚，但是據信，由於十二烷基苯 磺酸這種表面活性劑本身還可以作爲一種酸來酸化聚乙烯 醇，這將有利於聚乙稀醇的内部交聯，從而進一步提高聚 乙烯醇的防黏效果。在使用十二烷基苯磺酸鈉的時候，也 可以通過酸化來進一步提高聚乙烯醇塗層的防黏效果。 溶液的pH範圍在丨到14均可❶根據某些較佳的實施 方案，其中所述的組合物的pH值爲11〇，更佳爲25。酸 化時可以使用有機或無機酸，其巾較佳為續酸類的有機酸 表面活性劑，例如十二烷基苯磺酸。 可以根據具體情況選擇表面活性劑的用量以使塗層具 有顯著的高溫高濕老化防霧性能。當用量到達一定比例 20 201020281 5 ❹ 10 15 時，再增加表面活性劑的用量對高溫高濕老化防霧性能並 沒有顯著提高。因此，根據某些較佳的實施方案，其中按 聚合物重量爲100重量％計，陰離子表面活性劑的用量爲 i 重量㈣20重量％ ’更佳爲1.5重量％到15重量％。如 果陰離子表面活性劑的量過多，它們和聚乙稀醇之間的相 互作用會使溶液在PET表面鋪展的不好，從而影響塗層的 外觀。量太少’則達不到最好的高溫高濕老化防霧效果。 …根據某些較佳的實施方案，爲了同時達到很好的高溫 高濕老化防霧和抗黏的效果，適用於本發明的表面活性劑 可以是兩種或兩種以上不同的陰離子表面活性劑的組合， 其中至y種陰離子表面活性劑例如仲炫基續酸納主要用 來改善防霧性能，而其他種類的陰離子表面活性劑例如十 二烷基苯磺酸，主要用於提高塗層的抗黏性能。 根據某些較佳的實施方案，本發明的組合物中還含有 無毒或低毒性無機氧化物顆粒，例如二氧化矽、氧化鋅、 氧化紹’氧化錯’氧化辦，氧化錤，氧化鈦較佳之平均 粒仏爲1 150奈米的奈米級二氧化#。在聚乙稀醇和陰離 子表面活性劑構成的組合物中適當加入Si〇2的奈米顆粒可 以進步提尚本發明組合物的抗黏能力，使其高溫高濕老 化防霧性能同時達到最佳。二氧化矽可以以水溶液形式使 用。適用於本發明的二氧化矽，例如，可商購自Nak〇公 司。各種不同粒徑的Si〇2奈米顆粒都可適用於本發明的二 氧化矽，例如，購自Nalco公司的Si〇2奈米顆粒水溶液包 括’但不限於：U15(4nm)，2326(5nm)，U3〇 (8rlm)， 20 201020281 1030 (13 nm)，1050 (20 nm)，2327 (20 nm)，TX11561 (45 nm)，1060 (60 nm)和2329 (75 nm)。粒徑大小和奈米顆粒 的加入量對於塗層性能的影響非常大。大顆粒的奈米si〇2 抗黏效果更好。粒徑越大，需要加入的Si〇2量就越少。 5 e 10 15 ❹ 根據某些較佳的實施方案，本發明的組合物中按聚合 物重量爲100重量°/❶計’所述二氧化矽的用量爲5%到 60%。Si〇2的用量太低則抗黏效果的提高不夠顯著，用量 過高則會導致塗層發白’同時影響塗層的防霧性能的提高 程度。 根據某些較佳的實施方案，本發明的組合物中還含有 交聯劑，例如正矽酸乙酯或其預聚物，或者縮水甘油醚基 丙基二甲氧基石夕烧或其預聚物。交聯劑在本發明組合物中 用來提高其交聯度，從而增強塗層的物理性能，如提高塗 層耐濕擦的能力。爲了保證塗層在高溫高濕條件下的老化 防霧性能，一般此類交聯劑的用量不應超過聚合物例如聚 乙烯醇重量的2%。 對於本發明組合物中聚合物的濃度，沒有特別限制。 但是根據某些較佳的實施方案，聚合物佔所述組合物總重 量的3%到10%。 根據某些較佳的實施方案，本發明組合物中所述的聚 乙烯醇的醇解度爲60-100%，較佳為86%_1〇〇0/。。這是因爲 低醇解度的聚乙烯醇防水能力差。在高濕條件下塗層互相 接觸後容易出現互相黏連的情況。但是，低醇解度並不影 響塗層的南溫南濕老化防霧性能。 20 201020281 根據某些較佳的實施方案，本發明組合物中所述溶劑 較佳為水性溶劑，更佳爲水1以在水的基礎上加入一種 或多種其他的極性溶齡纽溶，所述其他的溶劑的例子 包括乙醇、曱醇、異丙醇、丙酮等。 5 10 15 ❹ 20 本發明還提供了一種薄膜，其包括基材和位於所述基 材至夕一個表面的至少一部分上的由本發明防霧塗層組合 物製成的乾燥黏附塗層《防霧塗層可在基材上進行單面或 者雙面的塗覆。 所述基材包括可見光區域内透明和半透明材料。例如 聚酯（如聚對苯二甲酸乙二醇酯（PET)、聚對苯二曱酸丁 二醇酯（PBT))，聚碳酸酯（PC)，烯丙基二甘醇碳酸 醋、聚丙烯酸酯（例如聚甲基丙烯酸曱酯）、聚苯乙烯、 聚颯樹脂、聚醚砜樹脂、環氧均聚物、環氧加成聚二胺類 高分子、環氧加成聚二醇類高分子、聚乙烯及其共聚物、 3复表面’纖維素醋’例如醋酸纖維素醋、丁酸纖維素g旨 等、玻璃、陶瓷、有機和無機複合表面等、以及上述材料 構成的混合物和層合物。 通常基材會以薄膜，板材或者塊狀材料的形式存在， 並且有可能是製品的一部分，例如眼科鏡、建築玻璃、裝 飾用玻璃邊框、車窗和擋風玻璃、保護眼睛的裝置，如手 術面具和面罩。如果需要，塗層可以只覆蓋製品的一部分， 例如只覆蓋面罩上與眼睛緊鄰的部位。基材可以是平的， 彎曲的或者各種形狀的。製品可以通過吹塑、澆鑄、樁 注塑等方法製造。 11 201020281 自聚對本發明薄臈巾所述基材選 醇醋(ΡΕΤ)、聚萘二甲酸乙二醇醋、 聚對本一甲g文丁一醇S旨（pbt彳 MBT)、聚碳酸酯（pc) 烴、聚苯乙烯、玻璃、聚甲其 眾甲基丙烯酸甲酯（ΡΜΜΛ)等透 明材料，及上述材料構成的 r結匕 珉的組合物。更佳爲聚對苯二甲酸Plastics Co. ; "IconolTM NP_70", available from BASF Corp.) and polyethylene/polypropylene glycol block copolymers (both can be "TetronicTM 1502 20 Block Copolymer Surfactant,""TetronicTM 908 Block Copolymer Surfactant" and "PluronicTM F38 Block Copolymer Surfactant, " from BASF, Corp.). Of course, any added wetting agent must be added in an amount that does not detract from the anti-fog properties of the coating. The wetting agent is usually used in an amount of less than about 0.1% by weight, based on the total weight of the coating composition, based on the amount of the cerium oxide nano-sized particles, preferably from about 0.003 to 201020281 and 0.05% by weight. Excessive surfactant or wetting agent can be removed by rinsing or by soaking the coated article in water. 5 参10 15 参 According to certain preferred embodiments, anionic surfactants suitable for use in the present invention include, but are not limited to, carboxylates, sulfates, squages (including mono- and di-ester salts), Fluorinated anionic surfactants and acid or sulfonate surfactants. Among them, preferred are sulfonic acid and sulfonate anionic surfactants. More preferably, it is a secondary alkyl sulfonate such as sodium secondary alkyl sulfonate, alkyl benzene sulfonic acid, such as dodecyl benzene sulfonic acid, alkyl benzene sulfonate, such as sodium dodecyl benzene sulfonate And succinate sulfonates such as hydrazine, 4-di(2-ethylhexyl)-sodium hydride. According to certain preferred embodiments, the present invention employs dodecylbenzenesulfonic acid and/or sodium dodecylbenzenesulfonate as an anionic surfactant. These two surfactants are particularly advantageous in terms of the anti-sticking effect of the proposed polyvinyl alcohol coating. While not wishing to be bound by theory, it is believed that since the surfactant of dodecylbenzenesulfonic acid itself can also be used as an acid to acidify polyvinyl alcohol, this will facilitate internal crosslinking of the polyethylene glycol. Thereby further improving the anti-adhesive effect of polyvinyl alcohol. When sodium dodecylbenzenesulfonate is used, the anti-adhesive effect of the polyvinyl alcohol coating can be further improved by acidification. The pH of the solution may range from 丨 to 14 according to certain preferred embodiments wherein the composition has a pH of 11 Torr, more preferably 25. An organic or inorganic acid may be used for the acidification, and the towel is preferably an acid-based organic acid surfactant such as dodecylbenzenesulfonic acid. The amount of the surfactant may be selected according to the specific conditions to impart significant high temperature and high humidity aging antifogging properties to the coating. When the dosage reaches a certain ratio of 20 201020281 5 ❹ 10 15 , the increase of the amount of surfactant does not significantly improve the anti-fog performance of high temperature and high humidity aging. Thus, according to certain preferred embodiments, the anionic surfactant is used in an amount of i by weight (four) 20% by weight', more preferably from 1.5% by weight to 15% by weight, based on 100% by weight of the polymer. If the amount of anionic surfactant is too large, the interaction between them and the polyethylene will cause the solution to spread poorly on the PET surface, thereby affecting the appearance of the coating. If the amount is too small, the best high temperature and high humidity aging anti-fog effect will not be achieved. According to certain preferred embodiments, the surfactant suitable for use in the present invention may be two or more different anionic surfactants in order to achieve good high temperature and high humidity aging antifogging and anti-sticking effects at the same time. a combination of y anionic surfactants such as succinyl sodium sulphate is mainly used to improve antifogging properties, while other types of anionic surfactants such as dodecyl benzene sulfonic acid are mainly used to improve the coating. Anti-adhesive properties. According to certain preferred embodiments, the composition of the present invention further comprises non-toxic or low-toxicity inorganic oxide particles, such as cerium oxide, zinc oxide, oxidized oxidized oxidized oxidized cerium, cerium oxide, and titanium oxide. The average particle size is 1 150 nm of nano-sized dioxide #. The appropriate addition of Si〇2 nanoparticles in the composition of the polyethylene glycol and the anionic surfactant can improve the anti-sticking ability of the composition of the present invention, and at the same time optimize the high-temperature, high-humidity and anti-fogging properties. Cerium dioxide can be used in the form of an aqueous solution. Cerium oxide suitable for use in the present invention is, for example, commercially available from Nak®. Various Si 2 nanoparticles having different particle diameters can be applied to the ceria of the present invention. For example, an aqueous solution of Si 2 nanoparticle obtained from Nalco Co., Ltd. includes, but is not limited to, U15 (4 nm), 2326 (5 nm). ), U3〇(8rlm), 20 201020281 1030 (13 nm), 1050 (20 nm), 2327 (20 nm), TX11561 (45 nm), 1060 (60 nm) and 2329 (75 nm). The particle size and the amount of nanoparticle added have a great influence on the properties of the coating. The large particle nano-si〇2 has a better anti-adhesive effect. The larger the particle size, the less the amount of Si〇2 that needs to be added. 5 e 10 15 ❹ According to certain preferred embodiments, the cerium oxide is present in the composition of the invention in an amount of from 5% to 60% by weight based on 100 parts by weight of the polymer. If the amount of Si〇2 is too low, the improvement of the anti-adhesive effect is not significant. If the amount is too high, the coating will be whitened and the antifogging property of the coating will be improved. According to certain preferred embodiments, the compositions of the present invention further comprise a crosslinking agent, such as ethyl ortho-nonanoate or a prepolymer thereof, or glycidyl ether propyl dimethoxylate or its prepolymerization. Things. Crosslinking agents are used in the compositions of the present invention to increase the degree of crosslinking, thereby enhancing the physical properties of the coating, such as increasing the ability of the coating to resist wet rubbing. In order to ensure the aging and antifogging properties of the coating under high temperature and high humidity conditions, the amount of such a crosslinking agent should generally not exceed 2% by weight of the polymer such as polyvinyl alcohol. There is no particular limitation on the concentration of the polymer in the composition of the present invention. However, according to certain preferred embodiments, the polymer comprises from 3% to 10% by weight of the total composition. According to certain preferred embodiments, the polyvinyl alcohol described in the composition of the invention has a degree of alcoholysis of from 60 to 100%, preferably from 86% to 1%. . This is because the low alcoholysis of polyvinyl alcohol is poor in water resistance. Under high-humidity conditions, the coatings tend to stick to each other after contact with each other. However, the low degree of alcoholysis does not affect the south temperature, humidity, and anti-fog properties of the coating. 20 201020281 According to certain preferred embodiments, the solvent in the composition of the invention is preferably an aqueous solvent, more preferably water 1 to add one or more other polar aging solutions on the basis of water. Examples of other solvents include ethanol, decyl alcohol, isopropanol, acetone, and the like. 5 10 15 ❹ 20 The present invention also provides a film comprising a substrate and a dry adhesive coating made of the anti-fog coating composition of the present invention on at least a portion of the surface of the substrate to the eve of the substrate. The coating can be applied to the substrate on one or both sides. The substrate comprises a transparent and translucent material in the visible region. For example, polyester (such as polyethylene terephthalate (PET), polybutylene terephthalate (PBT)), polycarbonate (PC), allyl diglycol carbonate, poly Acrylate (such as polymethyl methacrylate), polystyrene, polyfluorene resin, polyether sulfone resin, epoxy homopolymer, epoxy addition polydiamine polymer, epoxy addition polyglycol Polymer, polyethylene and copolymer thereof, 3 complex surface 'cellulose vinegar' such as cellulose acetate vinegar, cellulose butyrate, etc., glass, ceramic, organic and inorganic composite surface, etc., and mixtures of the above materials and Laminate. Usually the substrate will be in the form of a film, sheet or block material, and may be part of the product, such as ophthalmic mirrors, architectural glass, decorative glass bezels, windows and windshields, devices that protect the eyes, such as surgery. Masks and masks. If desired, the coating can cover only a portion of the article, such as only the portion of the mask that is immediately adjacent to the eye. The substrate can be flat, curved or of various shapes. The product can be produced by blow molding, casting, pile injection molding, and the like. 11 201020281 Self-polymerizing the substrate of the present invention, the base material is selected from the group consisting of alcoholic vinegar, polyethylene naphthalate, polyethylene terephthalate, pbt彳MBT, and polycarbonate. Pc) a transparent material such as a hydrocarbon, polystyrene, glass, polymethyl methacrylate or the like, and a composition of r crucible composed of the above materials. Polyterephthalic acid
Ci 一醇醋。 ’其包括根據本發明的薄 要防霧’尤其是親水防霧 本發明還提供了—種製品Ci a glycol vinegar. 'It includes a thin anti-fog according to the present invention', especially hydrophilic anti-fog. The present invention also provides an article of manufacture.
膜。本發明的製品適.用於所有需 的場合。 根據某些較佳的實施方案，本發明製品爲選自面罩、 眼鏡、廣告箱、展示櫥窗、測試試紙、攝像鏡射的形式。 更佳爲面罩，其包括但不限於醫療手術面罩、採礦用安全 面軍、焊接用防護面罩、冶煉廠用防護面罩。眼鏡也是較 佳的本發明製品，包括但不限於日常用眼鏡、游泳眼鏡、 5 實驗室用安全眼鏡、醫用眼鏡。 本發明之防霧塗層組合物可以採用常規方法製備，本 發明對其製備方法無任何限制。例如，可以將預定量的聚 合物或其任意濃度的溶液溶于溶劑中形成聚合物溶液然 2 後向其中加入需要量的陰離子表面活性劑和任選的無毒或 2〇低毒性氧化物顆粒，混合均勻，即製得本發明的防霧塗層 組合物。 下面，以聚乙烯醇作爲本發明組合物中聚合物組分和 水作爲溶劑組分爲例，對本發明防霧塗層組合物的製備方 法進行詳細說明。 12 201020281 (1)聚乙烯醇溶㈣製備：在攪拌條件下加入需要 =的1乙_至7()到8G攝氏度的去離子水中，保持授掉 直至聚乙稀醇溶解。 5 ⑶塗層組合物的製備：在需要量的聚乙稀醇溶液 I加入陰離子表面㈣劑和任選的各種添加劑，例如Si02 奈未級溶液等’保持祕至少三十分鐘即可得到本發明 的防霧塗層組合物。 將本發明防霧塗層組合物採用常規的塗敷方法，例如 線棒塗布'輕塗、簾式塗布、網棍塗布、喷塗、浸塗、氣 10刀式塗布等，塗在基材的至少一個表面的至少一部分上， 即可製得本發明的薄膜。較佳的塗敷方法包括線棒塗布、 網輥塗布、或氣刀式塗布以調節厚度。例如，將得到的本 發明塗層防霧、组合物溶液塗布在PET表面（例如用4μη1的線 棒），然後在指定溫度下烘乾適當長的時間，即可製得本 15 發明的薄膜。 爲了確保薄膜的均勻塗敷和潤濕，可以在塗敷前用電 暈放電或火焰處理方法氧化基材表面。能夠提高製品表面 能的其他方法包括使用化學預塗層處理如聚偏二氣乙烯 (PVDC)。爲了提高塗層和基材之間的結合力’可以根據需 2〇要選擇電暈和固化溫度。一般來說，t暈值和固化溫度越 高’得到的塗層和底材間的結合越好。電暈和固化溫度對 於塗層老化防霧性能沒有顯著影響。 將本發明的薄膜置於各種應用場合，即可得到本發明 的製品。 13 25 201020281 樣品製備及測試方法： 防霧性能測試 老化實驗是在50攝氏度，90%相對濕度的老化 5 e 10 15 Ο 行。防霧性能測試爲將樣品從老化箱中取出，深呼吸後 用嘴對著具有防霧塗層的薄膜面吹氣，沒有任何霧氣出現 在樣品表面爲通過標準。任何—點視覺可見的霧氣出現在 樣品表面都被判定爲不防霧，不論霧氣在樣品表面消失的 速度有多快。吹氣時人嘴離薄膜表面不應超過2釐米的距 離。 防黏測試 防黏測試也是在50攝氏度，90%相對濕度的老化箱中 進行。兩片薄膜疊放在一起（有防霧塗層的面互相接觸），上 面壓上六塊5cm X 10cm的不銹鋼板，其總重量大約爲22〇 克。 在從老化箱取出後樣品依然保持防霧（防黏）性能的 前提下’根據樣品在老化箱中可放置的最長時間制定了數 位化的防霧（防黏）性能標準。 在老化箱中最長放置時間 防霧性能 防黏性能 得分 得分 2小時以内 0 0 大於2小時，小於4小時 1 1 大於4小時，小於8小時 2 2 201020281 大於8小時，小於12小時 3 大於12小時，小於24小時 4-- ------- 4 大於24小時，小於48小時 5 5 大於48小時，小於72小時 6 6 大於72小時，小於96小時 十"~~ — ~Ί-- 大於96小時，小於120小時 8 8 大於120小時，小於144小時 9 9 大於144小時 10~' --—-- 10 實驗所用PET均來自上海紫城包membrane. The articles of the present invention are suitable for all occasions where they are needed. According to certain preferred embodiments, the article of the present invention is in the form of a mask, eyeglasses, advertising box, display window, test paper, camera lens. More preferred are masks including, but not limited to, medical surgical masks, mining safety surfaces, welding protective masks, and protective masks for smelters. Glasses are also preferred articles of the invention including, but not limited to, everyday glasses, swimming goggles, 5 laboratory safety glasses, medical glasses. The anti-fog coating composition of the present invention can be produced by a conventional method, and the preparation method of the present invention is not limited at all. For example, a predetermined amount of the polymer or a solution of any concentration thereof may be dissolved in a solvent to form a polymer solution, and then a desired amount of an anionic surfactant and optionally a non-toxic or 2-pure low toxicity oxide particle may be added thereto. The anti-fog coating composition of the present invention is obtained by uniformly mixing. Next, the preparation method of the anti-fog coating composition of the present invention will be described in detail by taking polyvinyl alcohol as a polymer component in the composition of the present invention and water as a solvent component. 12 201020281 (1) Polyvinyl alcohol solution (4) Preparation: Add 1 B_ to 7 () to 8 G Celsius in deionized water under stirring, and keep it until the polyethylene glycol is dissolved. 5 (3) Preparation of the coating composition: adding the anionic surface (tetra) agent and optionally various additives, such as SiO 2 nai solution, etc., in the required amount of the polyvinyl alcohol solution I to retain the secret for at least thirty minutes to obtain the present invention. Anti-fog coating composition. The anti-fog coating composition of the present invention is applied to a substrate by a conventional coating method such as wire coating, light coating, curtain coating, net coating, spray coating, dip coating, gas 10 knife coating, and the like. The film of the present invention can be obtained on at least a portion of at least one surface. Preferred coating methods include wire bar coating, web roll coating, or air knife coating to adjust the thickness. For example, the obtained coating anti-fog, composition solution of the present invention is coated on a PET surface (e.g., with a 4 μηη wire rod) and then dried at a specified temperature for a suitable length of time to obtain the film of the present invention. To ensure uniform coating and wetting of the film, the surface of the substrate can be oxidized by corona discharge or flame treatment prior to coating. Other methods that can increase the surface energy of the article include the use of chemical precoating processes such as polyvinylidene gas (PVDC). In order to increase the bonding force between the coating and the substrate, the corona and curing temperatures can be selected according to the requirements. In general, the higher the t halo value and the curing temperature, the better the bond between the resulting coating and the substrate. The corona and cure temperatures have no significant effect on the aging and anti-fog properties of the coating. The article of the present invention can be obtained by placing the film of the present invention in various applications. 13 25 201020281 Sample preparation and test methods: Anti-fog performance test The aging test is performed at 50 ° C, 90% relative humidity aging 5 e 10 15 Ο. The anti-fog performance test is to take the sample out of the aging box, and after deep breathing, blow the air against the surface of the film with the anti-fog coating, and no fog appears on the surface of the sample to pass the standard. Any point-visible fog appears on the surface of the sample to be judged as not anti-fog, no matter how fast the fog disappears on the surface of the sample. The mouth of the person should not exceed 2 cm from the surface of the film when blowing. Anti-stick test The anti-adhesion test is also carried out in an aging chamber at 50 degrees Celsius and 90% relative humidity. Two sheets of film are stacked together (the surfaces with anti-fog coating are in contact with each other), and six 5 cm X 10 cm stainless steel plates are pressed on the upper surface, and the total weight is about 22 gram. On the premise that the sample remains anti-fog (anti-adhesive) after being taken out of the aging box, the digital anti-fog (anti-stick) performance standard is established based on the maximum time the sample can be placed in the aging box. The longest placement time in the aging box Anti-fog performance Anti-stick performance score score within 2 hours 0 0 More than 2 hours, less than 4 hours 1 1 More than 4 hours, less than 8 hours 2 2 201020281 More than 8 hours, less than 12 hours 3 More than 12 hours , less than 24 hours 4-- ------- 4 greater than 24 hours, less than 48 hours 5 5 greater than 48 hours, less than 72 hours 6 6 greater than 72 hours, less than 96 hours ten "~~ — ~Ί-- More than 96 hours, less than 120 hours 8 8 more than 120 hours, less than 144 hours 9 9 more than 144 hours 10~' ----- 10 PET used in the experiment are from Shanghai Zichengbao
5 Φ 10 國上海）。所使用聚乙稀醇包括Nippon Gohsei公司（日本） 生産的GM-14和N-300。其中GM-14的醇解度爲 86.5%_89%，分子量介於44000和66000之間。N_300沾 醇解度爲98%-99%，分子量在66000以上。 除非特別指出，本發明中所有份數、比值、百分率# 以重量爲基準。 具體實施例 下面的實施例和對比實施例中採用的原料、其用途及 來源列舉如下： 辛基酚聚氧乙烯醚（Triton X-100，陶氏中國有限公 司，中國上海） 烷基二曱基卞基氣化銨的複配物（Bardac 208, Lonza 公司，瑞士） 10°/〇的D-吡喃葡萄糖，低聚物，癸基辛基葡萄糖 (BG-10，陶氏中國，中國上海） 15 15 201020281 氫化蓖麻油（PEG_40,上海協泰化工有限公司， 國上海） 脂肪族聚氧乙烯醚（AEO-7，陶氏由關 上 J八中國，中國上海） 5 10 15 20 N-油醯基多縮氨基酸@ (雷米邦A，上海威潔日用化 工有限公司，中國上海） 十二烷基苯磺酸（京帝化工，中國上海） 十二烷基苯磺酸鈉（米蘭化工，中國南亨） 十一烧基續酸納（上海盛衆精細化工有限公司，中 國上海） 仲烷基磺酸鈉（SAS60,上海諾泰化工有限公司，中 國上海） 1，4-二（2-乙基己基）-續酸鈉（GR_5N1，陶氏中國， 中國上海） 十二烷基硫酸鈉（上海協泰化工有限公司，中國上海） 十二烷基磷酸鉀（丹東金海精細化工有限公司，中 國遼寧省丹東市） 經甲基纖維素（分子量98000,上海嘉辰化工有限公 司’中國上海） 聚丙稀酸（分子量15000，金升化工有限公司，中國 河南省，新鄉市）5 Φ 10 countries Shanghai). The polyethylene glycol used includes GM-14 and N-300 produced by Nippon Gohsei Co., Ltd. (Japan). Among them, the degree of alcoholysis of GM-14 is 86.5%_89%, and the molecular weight is between 44000 and 66000. N_300 has a degree of alcoholysis of 98%-99% and a molecular weight of 66000 or more. All parts, ratios, percentages in the present invention are by weight unless otherwise indicated. DETAILED DESCRIPTION OF THE INVENTION The materials used in the following examples and comparative examples, their uses and sources are listed below: Octylphenol ethoxylate (Triton X-100, Dow China Ltd., Shanghai, China) Alkyldidecyl Ammonium-based vaporized ammonium compound (Bardac 208, Lonza, Switzerland) 10°/〇 D-glucopyranose, oligomer, decyl octyl glucose (BG-10, Dow China, Shanghai, China) 15 15 201020281 Hydrogenated castor oil (PEG_40, Shanghai Xietai Chemical Co., Ltd., Shanghai, China) Aliphatic polyoxyethylene ether (AEO-7, Dow by Guan JVIII China, Shanghai, China) 5 10 15 20 N-oil base Polyamino Acid @ (Remibang A, Shanghai Weijie Daily Chemical Co., Ltd., Shanghai, China) Dodecylbenzenesulfonic acid (Jingdi Chemical, Shanghai, China) Sodium Dodecylbenzenesulfonate (Milan Chemical, China) Nanheng) Eleven-based Sodium Hydroxide (Shanghai Shengzhong Fine Chemical Co., Ltd., Shanghai, China) Sodium Alkyl Sulfonate (SAS60, Shanghai Nuotai Chemical Co., Ltd., Shanghai, China) 1,4-two (2-B Benzyl)-sodium sulphate (GR_5N1, Dow China, Medium Shanghai) Sodium Dodecyl Sulfate (Shanghai Xietai Chemical Co., Ltd., Shanghai, China) Potassium Dodecyl Phosphate (Dandong Jinhai Fine Chemical Co., Ltd., Dandong City, Liaoning Province, China) Methylcellulose (molecular weight 98000, Shanghai Jiachen) Chemical Co., Ltd. 'Shanghai, China') Polyacrylic acid (molecular weight 15000, Jinsheng Chemical Co., Ltd., Xinxiang City, Henan Province, China)
對比實施例1:在10g3%的聚乙烯醇水溶液（GM-14 或者N-300)中加入250 mg的10%的辛基酚聚氧乙烯醚， 授拌30分鐘。將得到的溶液用4μιη的線棒塗布在ΡΕτ表 面’然後置於120攝氏度的烘箱中一分鐘。最終得到的PET 16 201020281 * 膜在50攝氏度，90%相對濕度的環境下老化防霧性能爲2。 對比實施例2 (陽離子表面活性劑）：在10g 7%的 聚乙烯醇水溶液 （GM-14或者N-300)中加入250 mg的 10%的烷基二甲基卞基氯化銨的複配物，攪拌30分鐘。將 5 得到的溶液用4μιη的線棒塗布在PET表面，然後置於120 攝氏度的烘箱中一分鐘.最終得到的PET膜在50攝氏度， 90%相對濕度的環境下老化防霧性能爲0。 對比實施例3 (非離子表面活性劑）：在10g 7%的 ® 聚乙烯醇水溶液 （GM-14或者N-300)中加入250 mg的 10 10%的D-吡喃葡萄糖，低聚物，癸基辛基葡萄糖攪拌30分 鐘。將得到的溶液用4μιη的線棒塗布在PET表面，然後置 於120攝氏度的烘箱中一分鐘。最終得到的PET膜在50 攝氏度，90%相對濕度的環境下老化防霧性能爲2。 對比實施例4 (非離子表面活性劑）：在10g 7%的 15 聚乙烯醇水溶液 （GM-14或者N-300)中加入250 mg的 10%的氫化蓖麻油，擾拌30分鐘。將得到的溶液用4μπι的 φ 線棒塗布在PET表面，然後置於120攝氏度的烘箱中一分 鐘。最終得到的PET膜在50攝氏度，90%相對濕度的環境 下老化防霧性能爲1。 20 對比實施例5 (非離子表面活性劑）：在10g 7%的 聚乙烯醇水溶液 （GM-14或者N-300)中加入250mg的 10%的脂肪族聚氧乙烯醚，攪拌30分鐘。將得到的溶液用 4μιη的線棒塗布在PET表面，然後置於120攝氏度的烘箱 中一分鐘。最終得到的PET膜具在50攝氏度，90%相對濕 17 201020281 * 度的環境下老化防霧性能爲2。 實施例1 (陰離子表面活性劑）：在10g 7%的聚乙 烯醇水溶液 （GM-14)中加入250mg的10%的十二烷基苯 5 確酸水溶液，撥拌30分鐘。將得到的溶液用4μηι的線棒塗 布在PET表面，然後置於120攝氏度的烘箱中一分鐘。最 終得到的PET膜具在50攝氏度，90%相對濕度的環境下老 化防霧性能爲6。 ⑩ 實施例2 (陰離子表面活性劑）：在10g 7%的聚乙 10 烯醇水溶液 （GM-14)中加入250mg的10%的十二烷基苯 績酸鈉水溶液，授拌30分鐘。將得到的溶液用4μιη的線棒 塗布在PET表面，然後置於120攝氏度的烘箱中一分鐘。 最終得到的PET膜具在50攝氏度，90%相對濕度的環境下 老化防霧性能爲6。 15 實施例3 (陰離子表面活性劑）：在10g 7%的聚乙 烯醇水溶液 （GM-14)中加入250mg的10%的十二烷基磺 _ 酸納水溶液，撥拌30分鐘。將得到的溶液用4μηι的線棒塗 布在PET表面，然後置於120攝氏度的烘箱中一分鐘。最 終得到的PET膜具在50攝氏度，90%相對濕度的環境下老 20 化防霧性能爲7。 實施例4 (陰離子表面活性劑）：在10g 7%的聚 乙烯醇水溶液 （GM-14或者N-300)中加入250mg的10% 的仲烷基磺酸鈉水溶液，攪拌30分鐘。將得到的溶液用4μιη 的線棒塗布在PET表面，然後置於120攝氏度的烘箱中一 25 分鐘。最終得到的PET膜具在50攝氏度，90%相對濕度的 201020281 ， 環境下老化防霧性能爲10。 實施例5 (陰離子表面活性劑）：在1〇g 7%的聚 乙烯醇水溶液（GM-14或者N-300)中加入250mg的10% 的1’4-二（2-乙基己基）·磺酸鈉水溶液，攪拌3〇分鐘。將 5 得到的溶液用4μιη的線棒塗布在PET表面，然後置於12〇 攝氏度的烘箱中一分鐘。最終得到的PET膜具在5〇攝氏 度，90%相對濕度的環境下老化防霧性能爲ι〇。 ® f施例1_5和對比實施例卜5中得到的組合物的防霧 1〇 性能概括於下表1。 表1Comparative Example 1: 250 mg of 10% octylphenol ethoxylate was added to 10 g of a 3% aqueous solution of polyvinyl alcohol (GM-14 or N-300) and mixed for 30 minutes. The resulting solution was coated on a ΡΕτ surface with a 4 μηη wire rod and then placed in an oven at 120 ° C for one minute. The resulting PET 16 201020281 * The film has an anti-fog performance of 2 at 50 ° C and 90% relative humidity. Comparative Example 2 (Cationic Surfactant): A blend of 250 mg of 10% alkyl dimethyl decyl ammonium chloride was added to 10 g of a 7% aqueous solution of polyvinyl alcohol (GM-14 or N-300). Stir for 30 minutes. The solution obtained by 5 was coated on a PET surface with a 4 μm wire rod, and then placed in an oven at 120 ° C for one minute. The finally obtained PET film had an anti-fog property of 0 at 50 ° C and 90% relative humidity. Comparative Example 3 (Nonionic Surfactant): 250 mg of 10 10% D-glucopyranose, an oligomer, was added to 10 g of a 7% aqueous solution of polyvinyl alcohol (GM-14 or N-300). The thioglycolyl glucose was stirred for 30 minutes. The resulting solution was coated on a PET surface with a 4 μm wire rod and then placed in an oven at 120 ° C for one minute. The resulting PET film had an anti-fog property of 2 at 50 ° C and 90% relative humidity. Comparative Example 4 (Nonionic Surfactant): 250 mg of 10% hydrogenated castor oil was added to 10 g of a 7% aqueous solution of 15 polyvinyl alcohol (GM-14 or N-300), and the mixture was stirred for 30 minutes. The resulting solution was coated on a PET surface with a 4 μm φ bar and placed in an oven at 120 ° C for one minute. The resulting PET film had an anti-fog property of 1 at 50 ° C and 90% relative humidity. 20 Comparative Example 5 (nonionic surfactant): 250 mg of 10% aliphatic polyoxyethylene ether was added to 10 g of a 7% aqueous solution of polyvinyl alcohol (GM-14 or N-300), and stirred for 30 minutes. The resulting solution was coated on a PET surface with a 4 μm wire rod and then placed in an oven at 120 ° C for one minute. The resulting PET film has an aging anti-fog performance of 2 at 50 degrees Celsius and 90% relative humidity 17 201020281 * degrees. Example 1 (Anionic surfactant): 250 mg of a 10% aqueous solution of dodecylbenzene was added to 10 g of a 7% aqueous solution of polyvinyl alcohol (GM-14), and the mixture was stirred for 30 minutes. The resulting solution was coated on a PET surface with a 4 μηη wire rod and placed in an oven at 120 ° C for one minute. The final PET film has an anti-fog performance of 6 at 50 degrees Celsius and 90% relative humidity. 10 Example 2 (Anionic surfactant): 250 mg of a 10% aqueous solution of sodium dodecyl benzoate was added to 10 g of a 7% aqueous solution of polyethylenol (GM-14), and the mixture was stirred for 30 minutes. The resulting solution was coated on a PET surface with a 4 μm wire rod and then placed in an oven at 120 ° C for one minute. The resulting PET film has an aging anti-fog performance of 6 at 50 degrees Celsius and 90% relative humidity. 15 Example 3 (anionic surfactant): 250 mg of a 10% aqueous solution of dodecylsulfonate was added to 10 g of a 7% aqueous solution of polyvinyl alcohol (GM-14), and the mixture was stirred for 30 minutes. The resulting solution was coated on a PET surface with a 4 μηη wire rod and placed in an oven at 120 ° C for one minute. The final PET film has an anti-fog performance of 7 in an environment of 50 degrees Celsius and 90% relative humidity. Example 4 (Anionic surfactant): 250 mg of a 10% aqueous solution of sodium secondary alkylsulfonate was added to 10 g of a 7% aqueous solution of polyvinyl alcohol (GM-14 or N-300), followed by stirring for 30 minutes. The resulting solution was coated on a PET surface with a 4 μm bar and placed in an oven at 120 ° C for 25 minutes. The resulting PET film has an anti-fog performance of 10 in the environment at 50 degrees Celsius and 90% relative humidity of 201020281. Example 5 (anionic surfactant): 250 mg of 10% 1'4-di(2-ethylhexyl) was added to 1 g of a 7% aqueous solution of polyvinyl alcohol (GM-14 or N-300). Aqueous sodium sulfonate solution was stirred for 3 minutes. The resulting solution of 5 was coated on a PET surface with a 4 μm wire rod and placed in an oven at 12 ° C for one minute. The resulting PET film has an aging anti-fog property of 5 〇 Celsius and 90% relative humidity. The anti-fogging properties of the compositions obtained in the Examples 1 to 5 and Comparative Examples 5 to 5 were summarized in Table 1 below. Table 1
防霧性 能 對比實施例1 對比實施例2 對比實施例3 對比實施例4 實施例 實施例2 實施例3 實施例4 實施例5 辛基盼聚氧乙烯喊 陽離子表面活性劑 活性劑 非離子表面活性劑 活性劑 陰離子表面活性劑 陰離子表面活性劑 陰離子表面活性劑 陰離子表面活性劑 陰離子表面活性劑 2 2 2 6 10To- 19 201020281 ' 由表1可見，本發明中採用了特定量的陰離子表面活 性劑的組合物與採用其他表面活性劑的組合物相比，防霧 性能有顯著性的提高。 5 實施例6 (陰離子表面活性劑）：在10g 7%的聚 乙烯醇水溶液 （GM-14或者N-300)中加入250mg的10% 的十二烷基硫酸鈉水溶液，攪拌30分鐘。將得到的溶液用 4μηι的線棒塗布在PET表面，然後置於120攝氏度的烘箱 ® 中一分鐘。最終得到的PET膜具在50攝氏度，90%相對濕 10 度的環境下老化防霧性能爲5。 實施例7 (陰離子表面活性劑）：在10g 7%的聚 乙烯醇水溶液 （GM-14或者N-300)中加入250mg的10% 的十二烷基磷酸鉀水溶液，攪拌30分鐘。將得到的溶液用 4μπι的線棒塗布在PET表面，然後置於120攝氏度的烘箱 15 中一分鐘。最終得到的PET膜具在50攝氏度，90%相對濕 度的環境下老化防霧性能爲4。 參 實施例8 (陰離子表面活性劑）：在10g 7%的聚 乙烯醇水溶液 （GM-14或者N-300)中加入250mg的10% 的N—油醯基多縮氨基酸鈉水溶液，攪拌30分鐘》將得到 20 的溶液用4μηι的線棒塗布在PET表面，然後置於120攝氏 度的烘箱中一分鐘。最終得到的PET膜具在50攝氏度，90% 相對濕度的環境下老化防霧性能爲4。 實施例9 (陰離子表面活性劑）：在10g 7%的聚 乙烯醇水溶液 （N-300)中加入250mg的10%的十二烷基 25 苯磺酸水溶液，攪拌30分鐘。將得到的溶液用4μιη的線棒 20 201020281 塗布在PET表面，然後置於120攝氏度的烘箱中一分鐘。 最終得到的PET膜具在50攝氏度，90%相對濕度的環境下 老化防霧性能爲10。 實施例10 (陰離子表面活性劑）：在l〇g 7%的聚 5 乙烯醇水溶液 （N-300)中加入250mg的10%的十二烷基 苯磺酸鈉水溶液，攪拌30分鐘。將得到的溶液用4μιη的線 棒塗布在PET表面，然後置於120攝氏度的烘箱中一分鐘。 最終得到的PET膜具在50攝氏度，90%相對濕度的環境下 ® <化防霧性能爲10。 10 實施例11 (陰離子表面活性劑）：在l〇g 7%的聚 乙烯醇水溶液 （N-300)中加入250mg的10%的十二烷基 磺酸鈉水溶液，攪拌30分鐘。將得到的溶液用4μηι的線棒 塗布在PET表面，然後置於120攝氏度的烘箱中一分鐘。 最終得到的PET膜具在50攝氏度，90%相對濕度的環境下 15 老化防霧性能爲9。 實施例12:在10g 3%的聚乙烯醇水溶液（GM-14) © 中加入100mg的10%的1，4 -二（2-乙基己基）-磺酸鈉水溶 液，攪拌30分鐘。將得到的溶液用4μιη的線棒塗布在PET 表面，然後置於120攝氏度的烘箱中一分鐘。最終得到的 20 PET膜具在50攝氏度，90%相對濕度的環境下老化防霧性 能爲10。 實施例13:在10g 7°/。的聚乙烯醇水溶液（GM-14)Anti-fog performance Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Example Example 2 Example 3 Example 4 Example 5 Octyl expectation polyoxyethylene cation cationic surfactant active agent nonionic surface active Agent Active Agent Anionic Surfactant Anionic Surfactant Anionic Surfactant Anionic Surfactant Anionic Surfactant 2 2 2 6 10To- 19 201020281 ' As can be seen from Table 1, a certain amount of anionic surfactant is used in the present invention. The composition has a significant improvement in anti-fog performance compared to compositions using other surfactants. 5 Example 6 (anionic surfactant): 250 mg of a 10% aqueous solution of sodium lauryl sulfate was added to 10 g of a 7% aqueous solution of polyvinyl alcohol (GM-14 or N-300), followed by stirring for 30 minutes. The resulting solution was coated on a PET surface with a 4 μηι wire rod and placed in an oven ® at 120 ° C for one minute. The resulting PET film has an aging anti-fog performance of 5 at 50 degrees Celsius and 90% relative humidity of 10 degrees. Example 7 (Anionic surfactant): 250 mg of a 10% aqueous potassium dodecyl phosphate solution was added to 10 g of a 7% aqueous solution of polyvinyl alcohol (GM-14 or N-300), followed by stirring for 30 minutes. The resulting solution was coated on a PET surface with a 4 μm wire rod and then placed in an oven 15 at 120 ° C for one minute. The resulting PET film has an aging anti-fog performance of 4 at 50 degrees Celsius and 90% relative humidity. Reference Example 8 (Anionic Surfactant): 250 mg of a 10% aqueous solution of N-oleyls-polyamino acid sodium was added to 10 g of a 7% aqueous solution of polyvinyl alcohol (GM-14 or N-300), and stirred for 30 minutes. The solution of 20 was coated on a PET surface with a 4 μηι wire rod and placed in an oven at 120 ° C for one minute. The resulting PET film has an anti-fog property of 4 at 50 degrees Celsius and 90% relative humidity. Example 9 (anionic surfactant): 250 mg of a 10% aqueous solution of dodecyl 25 benzenesulfonic acid was added to 10 g of a 7% aqueous solution of polyvinyl alcohol (N-300), followed by stirring for 30 minutes. The resulting solution was coated on a PET surface with a 4 μηη bar 20 201020281 and then placed in an oven at 120 ° C for one minute. The resulting PET film has an aging anti-fog performance of 10 at 50 degrees Celsius and 90% relative humidity. Example 10 (anionic surfactant): 250 mg of a 10% aqueous solution of sodium dodecylbenzenesulfonate was added to 1 g of a 7% aqueous solution of polyvinylidene alcohol (N-300), followed by stirring for 30 minutes. The resulting solution was coated on a PET surface with a 4 μm wire rod and then placed in an oven at 120 ° C for one minute. The resulting PET film has an anti-fog performance of 10 at 50 degrees Celsius and 90% relative humidity. 10 Example 11 (anionic surfactant): 250 mg of a 10% aqueous sodium dodecylsulfonate solution was added to 1 g of a 7% aqueous solution of polyvinyl alcohol (N-300), followed by stirring for 30 minutes. The resulting solution was coated on a PET surface with a 4 μηι wire rod and then placed in an oven at 120 ° C for one minute. The resulting PET film has an aging anti-fog performance of 9 at 50 degrees Celsius and 90% relative humidity. Example 12: 100 mg of a 10% aqueous solution of sodium 1,4-di(2-ethylhexyl)-sulfonate was added to 10 g of a 3% aqueous solution of polyvinyl alcohol (GM-14), and stirred for 30 minutes. The resulting solution was coated on a PET surface with a 4 μm wire rod and then placed in an oven at 120 ° C for one minute. The resulting 20 PET film has an anti-fog property of 10 at 50 degrees Celsius and 90% relative humidity. Example 13: at 10 g 7 ° /. Polyvinyl alcohol aqueous solution (GM-14)
中加入150mg的10%的1,4 -二（2-乙基己基）-磺酸鈉水溶 液，攪拌30分鐘。將得到的溶液用4μιη的線棒塗布在PET 21 201020281 ’ 表面，然後置於120攝氏度的烘箱中一分鐘。最終得到的 PET膜具在50攝氏度，90%相對濕度的環境下老化防霧性 能爲10。 實施例14:在10g 7%的聚乙烯醇水溶液（GM-14) 5 中加入300mg的10%的1，4 -二（2-乙基己基）-磺酸鈉水溶 液，攪拌30分鐘。將得到的溶液用4μιη的線棒塗布在PET 表面，然後置於120攝氏度的烘箱中一分鐘。最終得到的 PET膜具在50攝氏度，90%相對濕度的環境下老化防霧性 ® 能爲10。 10 實施例15:在10g 7%的聚乙烯醇水溶液（GM-14) 中加入350mg的10%的十二烷基苯磺酸水溶液，攪拌30 分鐘，溶液pH值爲2.5左右。將得到的溶液用4μιη的線棒 塗布在PET表面，然後置於120攝氏度的烘箱中一分鐘。 最終得到的PET膜具在50攝氏度，90%相對濕度的環境下 15 老化防黏性能爲4。 實施例16:在10g 10%的聚乙烯醇水溶液（GM-14) ❿ 中加入450mg的10%的十二烷基苯磺酸水溶液，攪拌30 分鐘，溶液pH值爲2左右。將得到的溶液用4μιη的線棒 塗布在PET表面，然後置於120攝氏度的烘箱中一分鐘。 20 最終得到的PET膜具在50攝氏度，90%相對濕度的環境下 老化防黏性能爲4。 實施例17:在10g 7%的聚乙烯醇水溶液（GM-14) 中加入350mg的10%的十二烷基苯磺酸鈉水溶液，用磷酸 將溶液pH值調至2，攪拌30分鐘。將得到的溶液用4μιη 22 201020281 • 的線棒塗布在PET表面，然後置於120攝氏度的烘箱中一 分鐘。最終得到的PET膜具在50攝氏度，90%相對濕度的 環境下老化防黏性能爲4。 實施例18:在10g 5%的N-300水溶液中加入400 mg 5 的10%的十二烷基苯磺酸鈉水溶液，攪拌30分鐘。將得到 的溶液用4μηι的線棒塗布在1.7KW電暈處理過的PET表 面，然後置於140攝氏度的烘箱中一分鐘。最終得到的防 霧PET膜在50攝氏度，90%的相對濕度下老化防霧性能爲 ® 10，老化防黏性能爲6。 10 實施例19: 在10g 5%的N-300水溶液中加入400 mg的10%的十二烷基苯磺酸水溶液，攪拌1分鐘。納米Si02 1115原液（粒徑4nm，濃度15%)用去離子水稀釋至5%， 並用磷酸酸化至pH==2,將6g酸化過的1115溶液加入前面 的N-300和十二烷基苯磺酸溶液中，攪拌30分鐘。將得到 15 的溶液用4μιη的線棒塗布在1.7KW電暈處理過的PET表 面，然後置於140攝氏度的烘箱中一分鐘。最終得到的防 φ 霧PET膜在50攝氏度，90%的相對濕度下老化防霧性能爲 7，老化防黏性能爲10。 實施例21 : 在10g 5%的N-300水溶液中加入400 20 mg的10%的十二烷基苯磺酸水溶液，攪拌1分鐘。奈米Si02 2326原液（粒徑5nm，濃度15%)用去離子水稀釋至5%， 並用磷酸酸化至pH2，將4g酸化過的2326溶液加入前面 的N-300和十二烷基苯磺酸溶液中，攪拌30分鐘。將得到 的溶液用4μιη的線棒塗布在1.7KW電暈處理過的PET表 23 201020281 • 面，然後置於140攝氏度的烘箱中一分鐘。最終得到的防 霧PET膜在50攝氏度，90%的相對濕度下老化防霧和防黏 性能均爲10。 實施例22 : 在10g 5%的N-300水溶液中加入400 5 mg的10%的十二烷基苯磺酸水溶液，攪拌1分鐘。奈米Si02 1130原液（粒徑8nm，濃度30%)用去離子水稀釋至5%， 並用磷酸酸化至pH2，將4g酸化過的1130溶液加入前面 的N-300和十二烷基苯磺酸溶液中，攪拌30分鐘。將得到 ® 的溶液用4μπι的線棒塗布在1.7KW電暈處理過的PET表 10 面，然後置於140攝氏度的烘箱中一分鐘。最終得到的防 霧PET膜在50攝氏度，90%的相對濕度下老化防霧和防黏 性能均爲10。 實施例22 : 在10g 5%的N-300水溶液中加入400 mg的10%的十二烷基苯磺酸水溶液，攪拌1分鐘。奈米Si02 15 1030原液（粒徑13nm,濃度30%)用去離子水稀釋至5%， 並用磷酸酸化至pH2，將3g酸化過的1030溶液加入前面 〇 的N-300和十二烷基苯磺酸溶液中，攪拌30分鐘。將得到 的溶液用4μπι的線棒塗布在1.7KW電暈處理過的PET表 面，然後置於140攝氏度的烘箱中一分鐘。最終得到的防 20 霧PET膜在50攝氏度，90%的相對濕度下老化防霧和防黏 性能均爲10。 實施例23 :在10g 5%的N-300水溶液中加入400 mg 的10%的十二烷基苯磺酸鈉水溶液，攪拌1分鐘。奈米Si02 2327原液（粒徑20nm，濃度40%)用去離子水稀釋至5%， 24 201020281 將2.5g的5% 2327溶液加入前面的N-300和十二烷基苯磺 酸鈉溶液中，攪拌30分鐘。將得到的溶液用4μιη的線棒塗 布在1.7KW電暈處理過的PET表面，然後置於140攝氏度 的烘箱中一分鐘。最終得到的PET膜在50攝氏度，90%的 5 相對濕度下老化防霧和防黏結果均爲10。 實施例24 :在10g 5%的N-300水溶液中加入400 mg 的10%的十二烷基苯磺酸鈉水溶液，攪拌1分鐘。奈米Si02 1050原液（粒徑20nm,濃度50%)用去離子水稀釋至5%， ’ 將2.5g的5% 1050溶液加入前面的N-300和十二烷基苯磺 10 酸鈉溶液中，攪拌30分鐘。將得到的溶液用4μιη的線棒塗 布在1.7KW電暈處理過的PET表面，然後置於140攝氏度 的烘箱中一分鐘。最終得到的PET膜在50攝氏度，90%的 相對濕度下老化防霧和防黏結果均爲10。 實施例25 :在10g 5%的N-300水溶液中加入400 mg 15 的10%的十二烷基苯磺酸鈉水溶液，攪拌1分鐘。奈米Si02 TX11561原液（粒徑45nm，濃度40%)用去離子水稀釋至 φ 5%， 將2g的5% TX11561溶液加入前面的N-300和十二 烷基苯磺酸鈉溶液中，攪拌30分鐘。將得到的溶液用4μηι 的線棒塗布在1.7KW電暈處理過的PET表面，然後置於 20 140攝氏度的烘箱中一分鐘。最終得到的PET膜在50攝氏 度，90%的相對濕度下老化防霧和防黏結果均爲10。 實施例26 :在10g 5%的N-300水溶液中加入400 mg 的10%的十二烷基苯磺酸鈉水溶液，攪拌1分鐘。奈米Si02 1060原液（粒徑60nm，濃度50%)用去離子水稀釋至5%， 25 201020281 • 將1.5g的5% 1060溶液加入前面的N-300和十二烷基苯磺 酸鈉溶液中，攪拌30分鐘。將得到的溶液用4μιη的線棒塗 布在1.7KW電暈處理過的PET表面，然後置於140攝氏度 的烘箱中一分鐘。最終得到的PET膜在50攝氏度，90%的 5 相對濕度下老化防霧和防黏結果均爲10。 實施例27 :在10g 5%的N-300水溶液中加入400 mg 的10%的十二烷基苯磺酸鈉水溶液，攪拌1分鐘。奈米Si02 2329原液（粒徑75nm，濃度40%)用去離子水稀釋至5%， _ 將lg的5°/。2329溶液加入前面的N-300和十二烷基苯磺酸 10 鈉溶液中，攪拌30分鐘。將得到的溶液用4μπι的線棒塗布 在1.7KW電暈處理過的PET表面，然後置於140攝氏度的 烘箱中一分鐘。最終得到的PET膜在50攝氏度，90%的相 對濕度下老化防霧和防黏結果均爲10。 實施例28 :在10g 7%的GM-14水溶液中加入400mg 15 的10%的1，4 -二（2-乙基己基）-磺酸鈉鹽水溶液和350mg 的10%的十二烷基苯磺酸，攪拌30分鐘。將得到的溶液用 φ 4μπι的線棒塗布在PET表面，然後置於120攝氏度的烘箱 中一分鐘。最終得到的防霧PET膜具有良好的老化防霧效 果，在50攝氏度，90%相對濕度的環境下老化防霧性能爲 20 10，老化抗黏性能爲4。 實施例29 :在10g 3%的GM-14水溶液中加入200 mg 的10%的仲烷基磺酸鈉水溶液和250 mg，10%的十二烷基 苯磺酸水溶液，攪拌30分鐘。將得到的溶液用4μιη的線棒 塗布在PET表面，然後置於120攝氏度的烘箱中一分鐘。 26 201020281 • 最終得到的防霧PET膜在50攝氏度，90%的相對濕度下老 化防霧性能爲10。老化抗黏性能爲4。 實施例30:在10g 10%的N-300水溶液中加入150 mg 的10%的十二烷基苯磺酸水溶液，攪拌1分鐘。奈米Si02 5 1115原液 （4 nm，15%)用去離子水稀釋至5%，並用磷酸 酸化至pH=2，將4g酸化過的1115溶液加入前面的N-300 和十二烷基苯磺酸溶液中，攪拌30分鐘。將得到的溶液用 4μιη的線棒塗布在1.7KW電暈處理過的PET表面，然後置 ® 於140攝氏度的烘箱中一分鐘。最終得到的防霧PET膜在 10 50攝氏度，90%的相對濕度下老化防霧爲10，老化抗黏性 能爲8。 實施例31:在10g 10%的N-300水溶液中加入150 mg 的10%的十二烷基苯磺酸水溶液，攪拌1分鐘。奈米Si02 1115原液 （4 nm，15%)用去離子水稀釋至5%，並用磷酸 15 酸化至pH=2，將5g酸化過的1115溶液加入前面的N-300 和十二烷基苯磺酸溶液中，攪拌30分鐘。將得到的溶液用 φ 4μιη的線棒塗布在1.7KW電暈處理過的PET表面，然後置 於140攝氏度的烘箱中一分鐘。最終得到的防霧PET膜在 50攝氏度，90%的相對濕度下老化防霧爲8,老化抗黏性能 20 爲 9。 實施例32:在10g 7%的N-300水溶液中加入400 mg 的10%的十二烷基苯磺酸水溶液，攪拌1分鐘。奈米Si02 2326原液 （5nm, 15%)用去離子水稀釋至5%，並用磷酸 酸化至pH=2，將4g酸化過的2326溶液加入前面的N-300 27 201020281 * • 和十二烷基苯磺酸溶液中，攪拌30分鐘。將得到的溶液用 4μηι的線棒塗布在1.7KW電暈處理過的PET表面，然後置 於140攝氏度的烘箱中一分鐘。最終得到的防霧PET膜在 50攝氏度，90%的相對濕度下老化防霧和防黏性能均爲10。 5 實施例33 : 在10g 3%的N-300水溶液中加入600 mg的10%的十二烷基苯磺酸水溶液，攪拌1分鐘。奈米Si02 2326原液（5nm, 15%)用去離子水稀釋至5%，並用磷酸 酸化至pH=2,將3.6g酸化過的2326溶液加入前面的N-300 ® 和十二烷基苯磺酸溶液中，攪拌30分鐘。將得到的溶液用 10 4μπι的線棒塗布在1.7KW電暈處理過的PET表面，然後置 於140攝氏度的烘箱中一分鐘。最終得到的防霧PET膜在 50攝氏度，90%的相對濕度下老化防霧和防黏性能均爲10。 實施例34 :在10g 10%的N-300水溶液中加入400 mg的10%的十二烷基苯磺酸鈉水溶液，攪拌1分鐘。奈米 15 Si02 2329原液（75nm，40%)用去離子水稀釋至5%， 將 lg的5% 2329溶液加入前面的N-300和十二烷基苯磺酸鈉 φ 溶液中，攪拌30分鐘。將得到的溶液用4μπι的線棒塗布在 1.7KW電暈處理過的PET表面，然後置於140攝氏度的烘 箱中一分鐘。最終得到的PET膜在50攝氏度，90%的相對 20 濕度下老化防霧和防黏結果均爲10。 實施例35:在10g 3%的N-300水溶液中加入400 〇^ 的10%的仲烷基磺酸鈉水溶液，攪拌1分鐘。奈米Si02 2329 原液（75nm，40%)用去離子水稀釋至5%，將2g的5% 2329 溶液加入前面的N-300和仲烷基磺酸鈉溶液中，攪拌30分 28 201020281 • 鐘。將得到的溶液用4μιη的線棒塗布在1.7KW電暈處理過 的PET表面，然後置於140攝氏度的烘箱中一分鐘。最終 得到的PET膜在50攝氏度，90%的相對濕度下老化防霧和 防黏結果均爲10。 5 實施例36 :在10g 5%的N-300水溶液中加入250mg 的10%的仲烷基磺酸鈉水溶液，用鹽酸將溶液酸化至pH=2, 在60攝氏度加熱攪拌60分鐘。將得到的溶液用4μηι的線 棒塗布在PET表面，然後置於120攝氏度的烘箱中30分 ❹ 鐘。最終得到的防霧PET膜可以經過一次濕擦就脫落。在 10 50攝氏度，90%相對濕度的環境下老化防霧性能爲10。 實施例37 :在10g 5%的N-300水溶液中加入250mg 的10%的仲烷基磺酸鈉水溶液和0.10g 10%正矽酸乙酯的 乙醇溶液，用鹽酸將溶液酸化至pH2， 在60攝氏度加熱 攪拌60分鐘。將得到的溶液用4μιη的線棒塗布在PET表 15 面，然後置於120攝氏度的烘箱中30分鐘。最終得到的防 霧PET膜可以經受5次濕擦而不脫落。在50攝氏度，90% 〇 相對濕度的環境下老化防霧性能爲7。 實施例38 :在10g 5°/。的N-300水溶液中加入250mg 的10%的仲烷基磺酸鈉水溶液和0.05g 10%正矽酸乙酯的 20 乙醇溶液，用鹽酸將溶液酸化至pH2， 在60攝氏度加熱 攪拌60分鐘。將得到的溶液用4μιη的線棒塗布在PET表 面，然後置於120攝氏度的烘箱中30分鐘。最終得到的防 霧PET膜可以經受3次濕擦而不脫落。在50攝氏度，90% 相對濕度的環境下老化防霧性能爲9。 29 201020281 5 Ο ίο 15 ❹ 20 實施例39:在10g 10%的GM-14水溶液中加入300mg的 10%的仲烷基磺酸鈉水溶液，攪拌30分鐘。將得到的溶液 用4μπι的線棒塗布聚碳酸酯 （PC)表面，然後置於120 攝氏度的烘箱中一分鐘。最終得到的防霧PC膜具有良好的 老化防霧效果，在50攝氏度，90%相對濕度的環境下老化 防霧性能爲10。 實施例40:在10g 5%的N-300水溶液中加入400 mg 的10%的十二烷基苯磺酸鈉水溶液，攪拌1分鐘。奈米Si02 2329原液（75nm，40%)用去離子水稀釋至5%， 將1.5g 的5% 2329溶液加入前面的N-300和十二烷基苯磺酸鈉溶 液中，攪拌30分鐘。將得到的溶液用4μπι的線棒塗布在 1.7KW電暈處理過的聚礙酸酯表面，然後置於140攝氏度 的烘箱中一分鐘。最終得到的PC膜在50攝氏度，90%的 相對濕度下老化防霧和防黏結果均爲10。 實施例41 :在10g 3%的GM-14水溶液中加入200mg 的10%的仲烷基磺酸鈉水溶液，攪拌30分鐘。將得到的溶 液用4μιη的線棒塗布在玻璃表面，然後置於120攝氏度的 烘箱中一分鐘。最終得到的玻璃具有良好的老化防霧效 果，在50攝氏度，90%相對濕度的環境下老化防霧性能爲 10 ° 實施例42 :在10g 5%的羥甲基纖維素水溶液中加入 150 mg的10%的仲烷基磺酸鈉水溶液，攪拌1分鐘。將得 到的溶液用4μπι的線棒塗布在PET表面，然後置於120攝 氏度的烘箱中一分鐘。最終得到的PET膜在50攝氏度，90% 30 201020281 的相對濕度下老化防霧結果爲10。 5150 mg of a 10% aqueous solution of sodium 1,4-bis(2-ethylhexyl)sulfonate was added thereto, and the mixture was stirred for 30 minutes. The resulting solution was coated on a PET 21 201020281' surface with a 4 μm wire rod and then placed in an oven at 120 ° C for one minute. The resulting PET film has an anti-fog property of 10 at 50 degrees Celsius and 90% relative humidity. Example 14: 300 mg of a 10% aqueous solution of sodium 1,4-bis(2-ethylhexyl)-sulfonate was added to 10 g of a 7% aqueous solution of polyvinyl alcohol (GM-14) 5 and stirred for 30 minutes. The resulting solution was coated on a PET surface with a 4 μm wire rod and then placed in an oven at 120 ° C for one minute. The resulting PET film has an anti-fog property of 10 at 50 degrees Celsius and 90% relative humidity. 10 Example 15: 350 mg of a 10% aqueous solution of dodecylbenzenesulfonic acid was added to 10 g of a 7% aqueous solution of polyvinyl alcohol (GM-14), and the mixture was stirred for 30 minutes, and the pH of the solution was about 2.5. The resulting solution was coated on a PET surface with a 4 μm wire rod and then placed in an oven at 120 ° C for one minute. The resulting PET film has an aging anti-adhesive property of 4 at 50 degrees Celsius and 90% relative humidity. Example 16: 450 mg of a 10% aqueous solution of dodecylbenzenesulfonic acid was added to 10 g of a 10% aqueous solution of polyvinyl alcohol (GM-14), and the mixture was stirred for 30 minutes, and the pH of the solution was about 2. The resulting solution was coated on a PET surface with a 4 μm wire rod and then placed in an oven at 120 ° C for one minute. 20 The final PET film has an aging anti-adhesive property of 4 at 50 °C and 90% relative humidity. Example 17: 350 mg of a 10% aqueous solution of sodium dodecylbenzenesulfonate was added to 10 g of a 7% aqueous solution of polyvinyl alcohol (GM-14), and the pH of the solution was adjusted to 2 with phosphoric acid and stirred for 30 minutes. The resulting solution was coated on a PET surface with a wire rod of 4 μιη 22 201020281 • and placed in an oven at 120 ° C for one minute. The resulting PET film has an aging anti-adhesive property of 4 at 50 degrees Celsius and 90% relative humidity. Example 18: 400 mg of a 10% aqueous solution of sodium dodecylbenzenesulfonate was added to 10 g of a 5% aqueous N-300 solution and stirred for 30 minutes. The resulting solution was coated on a 1.7 KW corona treated PET surface with a 4 μηι wire rod and placed in an oven at 140 ° C for one minute. The resulting anti-fog PET film has an anti-fog performance of +10 at 50 °C and 90% relative humidity, and an aging anti-sticking performance of 6. 10 Example 19: 400 mg of a 10% aqueous solution of dodecylbenzenesulfonic acid was added to 10 g of a 5% N-300 aqueous solution and stirred for 1 minute. The nano-SiO 2 1115 stock solution (particle size 4 nm, concentration 15%) was diluted to 5% with deionized water, acidified to pH==2 with phosphoric acid, and 6 g of the acidified 1115 solution was added to the previous N-300 and dodecylbenzene. Stir in the sulfonic acid solution for 30 minutes. The resulting solution of 15 was coated on a 1.7 KW corona treated PET surface with a 4 μm bar and placed in an oven at 140 ° C for one minute. The resulting anti-φ fog PET film has an anti-fog property of 50 at 50 ° C and 90% relative humidity, and the aging anti-adhesive property is 10. Example 21: 400 20 mg of a 10% aqueous solution of dodecylbenzenesulfonic acid was added to 10 g of a 5% N-300 aqueous solution and stirred for 1 minute. Nano SiO 2 2326 stock solution (particle size 5 nm, concentration 15%) was diluted to 5% with deionized water and acidified to pH 2 with phosphoric acid. 4 g of acidified 2326 solution was added to the previous N-300 and dodecylbenzene sulfonic acid. Stir in the solution for 30 minutes. The resulting solution was coated on a 1.7 KW corona treated PET sheet with a 4 μιη bar bar and placed in an oven at 140 ° C for one minute. The resulting anti-fog PET film has an anti-fog and anti-stick property of 10 at 50 degrees Celsius and 90% relative humidity. Example 22: 400 5 mg of a 10% aqueous solution of dodecylbenzenesulfonic acid was added to 10 g of a 5% N-300 aqueous solution, and stirred for 1 minute. Nano SiO 2 1130 stock solution (particle size 8 nm, concentration 30%) was diluted to 5% with deionized water and acidified to pH 2 with phosphoric acid. 4 g of acidified 1130 solution was added to the previous N-300 and dodecylbenzene sulfonic acid. Stir in the solution for 30 minutes. The solution obtained from ® was coated on a 1.7 KW corona treated PET sheet with a 4 μm bar and placed in an oven at 140 ° C for one minute. The resulting anti-fog PET film has an anti-fog and anti-stick property of 10 at 50 degrees Celsius and 90% relative humidity. Example 22: 400 mg of a 10% aqueous solution of dodecylbenzenesulfonic acid was added to 10 g of a 5% N-300 aqueous solution, and stirred for 1 minute. Nano SiO 2 15 1030 stock solution (particle size 13nm, concentration 30%) diluted to 5% with deionized water, acidified to pH 2 with phosphoric acid, 3g acidified 1030 solution was added to the former 〇N-300 and dodecyl benzene Stir in the sulfonic acid solution for 30 minutes. The resulting solution was coated on a 1.7 KW corona treated PET surface with a 4 μm bar and placed in an oven at 140 ° C for one minute. The resulting anti-fog PET film has an anti-fog and anti-stick property of 10 at 50 degrees Celsius and 90% relative humidity. Example 23: 400 mg of a 10% aqueous solution of sodium dodecylbenzenesulfonate was added to 10 g of a 5% aqueous solution of N-300, and the mixture was stirred for 1 minute. Nano Si02 2327 stock solution (particle size 20nm, concentration 40%) diluted to 5% with deionized water, 24 201020281 2.5g of 5% 2327 solution was added to the previous N-300 and sodium dodecyl benzene sulfonate solution Stir for 30 minutes. The resulting solution was coated on a 1.7 KW corona treated PET surface with a 4 μm bar and placed in an oven at 140 ° C for one minute. The resulting PET film had an anti-fog and anti-sticking result of 10 at 50 degrees Celsius and 90% relative humidity. Example 24: 400 mg of a 10% aqueous solution of sodium dodecylbenzenesulfonate was added to 10 g of a 5% N-300 aqueous solution, and stirred for 1 minute. Nano Si02 1050 stock solution (particle size 20nm, concentration 50%) diluted to 5% with deionized water, '2.5 g of 5% 1050 solution was added to the previous N-300 and sodium dodecylbenzenesulfonate 10 sodium solution Stir for 30 minutes. The resulting solution was coated on a 1.7 KW corona treated PET surface with a 4 μm bar and placed in an oven at 140 ° C for one minute. The resulting PET film had an anti-fog and anti-sticking result of 10 at 50 degrees Celsius and 90% relative humidity. Example 25: 400 g of 15% aqueous 10% sodium dodecylbenzenesulfonate solution was added to 10 g of a 5% N-300 aqueous solution, and stirred for 1 minute. Nano Si02 TX11561 stock solution (particle size 45nm, concentration 40%) diluted to φ 5% with deionized water, 2g of 5% TX11561 solution was added to the previous N-300 and sodium dodecyl benzene sulfonate solution, stirring 30 minutes. The resulting solution was coated on a 1.7 KW corona treated PET surface with a 4 μηι wire rod and placed in an oven at 20 140 ° C for one minute. The resulting PET film had an anti-fog and anti-sticking result of 10 at 50 ° C and 90% relative humidity. Example 26: 400 mg of a 10% aqueous solution of sodium dodecylbenzenesulfonate was added to 10 g of a 5% aqueous N-300 solution and stirred for 1 minute. Nano Si02 1060 stock solution (particle size 60nm, concentration 50%) diluted to 5% with deionized water, 25 201020281 • Add 1.5g of 5% 1060 solution to the previous N-300 and sodium dodecyl benzene sulfonate solution Stir for 30 minutes. The resulting solution was coated on a 1.7 KW corona treated PET surface with a 4 μm bar and placed in an oven at 140 ° C for one minute. The resulting PET film had an anti-fog and anti-sticking result of 10 at 50 degrees Celsius and 90% relative humidity. Example 27: 400 mg of a 10% aqueous solution of sodium dodecylbenzenesulfonate was added to 10 g of a 5% aqueous N-300 solution and stirred for 1 minute. The nano-SiO 2 2329 stock solution (particle size 75 nm, concentration 40%) was diluted to 5% with deionized water, _ 5 ° / lg. The 2329 solution was added to the previous N-300 and sodium dodecylbenzenesulfonic acid 10 sodium solution and stirred for 30 minutes. The resulting solution was coated on a 1.7 KW corona treated PET surface with a 4 μm bar and placed in an oven at 140 ° C for one minute. The resulting PET film had an anti-fog and anti-sticking result of 10 at 50 degrees Celsius and 90% relative humidity. Example 28: 400 mg of 15% aqueous solution of 10% 1,4-di(2-ethylhexyl)-sulfonate and 350 mg of 10% dodecylbenzene were added to 10 g of a 7% aqueous solution of GM-14. The sulfonic acid was stirred for 30 minutes. The resulting solution was coated on a PET surface with a wire rod of φ 4 μm and placed in an oven at 120 ° C for one minute. The final anti-fog PET film has good aging anti-fog effect, and the anti-fog property is 20 10 at 50 ° C and 90% relative humidity, and the aging anti-adhesive property is 4. Example 29: 200 g of a 10% aqueous solution of sodium secondary alkylsulfonate and 250 mg of a 10% aqueous solution of dodecylbenzenesulfonic acid were added to 10 g of a 3% aqueous solution of GM-14, and stirred for 30 minutes. The resulting solution was coated on a PET surface with a 4 μm wire rod and then placed in an oven at 120 ° C for one minute. 26 201020281 • The final anti-fog PET film has an anti-fog performance of 10 at 50 degrees Celsius and 90% relative humidity. The aging anti-adhesive property is 4. Example 30: 150 mg of a 10% aqueous solution of dodecylbenzenesulfonic acid was added to 10 g of a 10% aqueous solution of N-300 and stirred for 1 minute. Nano SiO 2 5 1115 stock solution (4 nm, 15%) was diluted to 5% with deionized water and acidified to pH = 2 with phosphoric acid. 4 g of acidified 1115 solution was added to the previous N-300 and dodecylbenzene sulfonate. Stir in the acid solution for 30 minutes. The resulting solution was coated on a 1.7 KW corona treated PET surface with a 4 μηη wire rod and placed in an oven at 140 ° C for one minute. The resulting anti-fog PET film had an anti-fog of 10 at 10 50 degrees Celsius and 90% relative humidity, and an aging anti-sticking property of 8. Example 31: 150 mg of a 10% aqueous solution of dodecylbenzenesulfonic acid was added to 10 g of a 10% aqueous solution of N-300 and stirred for 1 minute. Nano Si02 1115 stock solution (4 nm, 15%) was diluted to 5% with deionized water and acidified to pH=2 with phosphoric acid 15 and 5 g of acidified 1115 solution was added to the previous N-300 and dodecylbenzenesulfonate. Stir in the acid solution for 30 minutes. The resulting solution was coated on a 1.7 KW corona treated PET surface with a wire rod of φ 4 μηη, and then placed in an oven at 140 ° C for one minute. The final anti-fog PET film has an anti-fog of 8 at 50 °C and 90% relative humidity, and an aging anti-sticking property of 20 of 9. Example 32: 400 mg of a 10% aqueous solution of dodecylbenzenesulfonic acid was added to 10 g of a 7% aqueous solution of N-300 and stirred for 1 minute. Nano SiO 2 2326 stock solution (5 nm, 15%) was diluted to 5% with deionized water and acidified to pH = 2 with phosphoric acid. 4 g of acidified 2326 solution was added to the previous N-300 27 201020281 * • and dodecyl Stir in the benzenesulfonic acid solution for 30 minutes. The resulting solution was coated on a 1.7 KW corona treated PET surface with a 4 μηη wire rod and placed in an oven at 140 ° C for one minute. The resulting anti-fog PET film has an anti-fog and anti-stick property of 10 at 50 degrees Celsius and 90% relative humidity. 5 Example 33: 600 g of a 10% aqueous solution of dodecylbenzenesulfonic acid was added to 10 g of a 3% N-300 aqueous solution and stirred for 1 minute. Nano SiO 2 2326 stock solution (5 nm, 15%) was diluted to 5% with deionized water and acidified to pH = 2 with phosphoric acid. 3.6 g of acidified 2326 solution was added to the previous N-300 ® and dodecylbenzene sulfonate. Stir in the acid solution for 30 minutes. The resulting solution was coated on a 1.7 KW corona treated PET surface with a wire rod of 10 4 μm, and then placed in an oven at 140 ° C for one minute. The resulting anti-fog PET film has an anti-fog and anti-stick property of 10 at 50 degrees Celsius and 90% relative humidity. Example 34: 400 mg of a 10% aqueous solution of sodium dodecylbenzenesulfonate was added to 10 g of a 10% aqueous solution of N-300 and stirred for 1 minute. Nano 15 SiO 2 2329 stock solution (75 nm, 40%) diluted to 5% with deionized water, 5% 5% 2329 solution was added to the previous N-300 and sodium dodecyl benzene sulfonate φ solution, stirred for 30 minutes . The resulting solution was coated on a 1.7 KW corona treated PET surface with a 4 μm bar and placed in an oven at 140 ° C for one minute. The resulting PET film had an anti-fog and anti-sticking result of 10 at 50 degrees Celsius and 90% relative humidity. Example 35: 400 g of a 10% aqueous solution of sodium secondary alkylsulfonate was added to 10 g of a 3% N-300 aqueous solution and stirred for 1 minute. Nano SiO 2 2329 stock solution (75nm, 40%) diluted to 5% with deionized water, 2g of 5% 2329 solution was added to the previous N-300 and sodium sulfonate solution, stirring 30 minutes 28 201020281 • Clock . The resulting solution was coated on a 1.7 KW corona treated PET surface with a 4 μm bar and placed in an oven at 140 ° C for one minute. The resulting PET film had an anti-fog and anti-sticking result of 10 at 50 degrees Celsius and 90% relative humidity. 5 Example 36: 250 mg of a 10% aqueous solution of sodium secondary alkylsulfonate was added to 10 g of a 5% aqueous solution of N-300, and the solution was acidified to pH = 2 with hydrochloric acid, and stirred under heating at 60 ° C for 60 minutes. The resulting solution was coated on a PET surface with a 4 μηη wire rod and placed in an oven at 120 ° C for 30 minutes. The resulting anti-fog PET film can be peeled off after a wet rub. The aging anti-fog performance is 10 at 10 50 degrees Celsius and 90% relative humidity. Example 37: 250 g of a 10% aqueous solution of sodium secondary alkyl sulfonate and 0.10 g of 10% ethyl ortho-nonanoate in ethanol were added to 10 g of a 5% N-300 aqueous solution, and the solution was acidified to pH 2 with hydrochloric acid. Heat and stir for 60 minutes at 60 degrees Celsius. The resulting solution was coated on a PET surface with a 4 μm wire rod and then placed in an oven at 120 ° C for 30 minutes. The finally obtained antifogging PET film can withstand 5 wet rubs without falling off. The aging anti-fog performance is 7 at 50 degrees Celsius and 90% 相对 relative humidity. Example 38: at 10 g 5 ° /. To the N-300 aqueous solution, 250 mg of a 10% aqueous solution of sodium secondary alkylsulfonate and 0.05 g of a 10% solution of ethyl ortho-nonanoate in 20 ethanol were added, and the solution was acidified to pH 2 with hydrochloric acid, and stirred at 60 ° C for 60 minutes. The resulting solution was coated on a PET surface with a 4 μm wire bar and then placed in an oven at 120 ° C for 30 minutes. The finally obtained antifogging PET film can withstand 3 wet rubs without falling off. The aging anti-fog performance is 9 at 50 degrees Celsius and 90% relative humidity. 29 201020281 5 Ο ίο 15 ❹ 20 Example 39: 300 mg of a 10% aqueous solution of sodium secondary alkylsulfonate was added to 10 g of a 10% aqueous solution of GM-14, and stirred for 30 minutes. The resulting solution was coated on a polycarbonate (PC) surface with a 4 μm bar and placed in an oven at 120 ° C for one minute. The resulting anti-fog PC film has a good anti-fog effect, and the anti-fog property is 10 at 50 degrees Celsius and 90% relative humidity. Example 40: 400 mg of a 10% aqueous solution of sodium dodecylbenzenesulfonate was added to 10 g of a 5% aqueous N-300 solution and stirred for 1 minute. The nano-SiO 2 2329 stock solution (75 nm, 40%) was diluted to 5% with deionized water, and 1.5 g of a 5% 2329 solution was added to the previous solution of N-300 and sodium dodecylbenzenesulfonate, and stirred for 30 minutes. The resulting solution was coated on a 1.7 KW corona treated agglomerate surface with a 4 μm bar and placed in an oven at 140 ° C for one minute. The resulting PC film had an anti-fog and anti-sticking result of 10 at 50 degrees Celsius and 90% relative humidity. Example 41: 200 mg of a 10% aqueous solution of sodium secondary alkylsulfonate was added to 10 g of a 3% aqueous solution of GM-14, followed by stirring for 30 minutes. The resulting solution was coated on a glass surface with a 4 μm wire rod and then placed in an oven at 120 ° C for one minute. The resulting glass has a good aging anti-fog effect, and the anti-fog property is 10 ° at 50 ° C and 90% relative humidity. Example 42: 150 mg is added to 10 g of a 5% aqueous solution of hydroxymethylcellulose. A 10% aqueous solution of sodium secondary alkylsulfonate was stirred for 1 minute. The resulting solution was coated on a PET surface with a 4 μm wire rod and placed in an oven at 120 ° C for one minute. The resulting PET film was aged to an anti-fog of 10 at a relative humidity of 50 degrees Celsius and 90% 30 201020281. 5
實施例43:在10g 10°/。的聚丙烯酸水溶液中加入400 mg的1〇%的仲烷基磺酸鈉水溶液，攪拌1分鐘。將得到的 溶液用4μιη的線棒塗布在PET表面，然後置於120攝氏度 的烘箱中一分鐘。最終得到的PET膜在50攝氏度，9〇%的 相對濕度下老化防霧結果爲10。 舉例而已，本發明所 所述為準，而非僅限 上述實施例僅係為了方便說明而 主張之權利範圍自應以申請專利範圍 於上述實施例。 【圖式簡單說明】 無 【主要元件符號說明】 15 無 餐 31Example 43: at 10 g 10 ° /. 400 mg of a 1% aqueous solution of sodium secondary alkylsulfonate was added to the aqueous polyacrylic acid solution, and the mixture was stirred for 1 minute. The resulting solution was coated on a PET surface with a 4 μm wire rod and placed in an oven at 120 ° C for one minute. The resulting PET film had an anti-fog result of 10 at 50 ° C and a relative humidity of 9 %. The present invention is intended to be limited, and not limited to the foregoing embodiments, which are intended to be illustrative only. [Simple diagram description] None [Main component symbol description] 15 No Meal 31
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111574960A (en) * | 2020-05-12 | 2020-08-25 | 浙江优亿医疗器械有限公司 | Formula and preparation method of antifogging liquid |
| CN117089179A (en) * | 2023-09-11 | 2023-11-21 | 佛山赛和薄膜科技有限公司 | High-transmittance low-fog optical base film and preparation method thereof |
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2008
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111574960A (en) * | 2020-05-12 | 2020-08-25 | 浙江优亿医疗器械有限公司 | Formula and preparation method of antifogging liquid |
| CN117089179A (en) * | 2023-09-11 | 2023-11-21 | 佛山赛和薄膜科技有限公司 | High-transmittance low-fog optical base film and preparation method thereof |
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