TW200907139A - Fabric care compositions - Google Patents
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200907139 九、發明說明: 【發明所屬之技術領域】 本括具有織物護理特性之聚胺基曱 物。本發明亦提供包括洗膝劑及織物軟化劑 、、口 合物,該等織物軟化劑包括聚胺 "濩理組 【先前技術】 基甲酸酿脲組合物。 ==了於添加至洗務劑中以賦予可物 r 減少靜電吸附、賦予令人愉悦 于… 少敏折並且使烫烫更容易… 減^、乾燥時間、減 洗-後隨時間=。然而’此等特性之益處通常在 ==組份係基於稱為四級錄化合物之長鏈脂肪 =“質上係陽離子性。因此,為防止與實質上可 洗或乾燥期間才引入織物軟=望之反應,通常在織物沖 時力 =少織物洗縣之時間及費用’業内需要可與洗務劑同 合物相濩理組合物。業内亦需要能使與織物軟化組 %貫體化及易於護理之各種益處之持續時間 卞以延長的織物護理組合物。 【發明内容】 脲本=提供-呈粉末或水性分散液形式之聚胺基甲酸 供織物洗峨織物軟化劑組合物組合使用可提 在—實施例中,織物護理組合物係、呈包括聚胺基甲酸酿 123499.doc 200907139 脲聚合物及水之非離子成膜分散液形式。該聚合物係預聚 物與作為鏈延長劑之水的反應產物’其中該預聚物係—種 二醇或數種二醇之混合物與多異氰酸酯(例如4,4,-亞甲基 雙(苯基異氰酸_))之反應產物。 另一實施例係一包括水及聚胺基甲酸酯脲聚合物之非離 子非成膜分散液。該聚合物係預聚物與鏈延長劑(例如二 胺鏈延長劑 '水及其組合)之反應產物,其中該預聚物係 二醇(多元醇)或二醇混合物與多異氰酸酯(例如4,4,_亞甲基 雙(本基異亂酸g旨))之反應產物。然後可將該聚合物過渡並 研磨或喷霧乾燥以提供一粉末。 又一實施例提供一延長織物或衣物上香味或香氣實體化 之方法。§玄方法包括使織物或衣物接觸一香油及呈粉末或 水性分散液形式之聚胺基甲酸酯脲組合物。該接觸可以多 種途徑發生,其包括(但不限於)在洗滌及/或乾燥織物前將 香油及聚胺基甲酸酯脲添加至洗滌劑或織物軟化劑中、直 接將其添加至洗滌用水中、或在沖洗循環期間將其直接或 與織物軟化劑組合物組合引入。 又一實施例提供一種為織物或衣物提供期望特性的方 法。該方法包括使織物接觸呈粉末或水性分散液形式之聚 胺基甲酸醋脲。可賦予織物之所期望特性包括(但不限於) 形狀保持、易護理(即,易熨烫)、及抗站污特性。 【實施方式】 本文所用術語"粉末”意指由微細固體粒子之鬆散團塊組 成之顆粒材料,該等固體粒子之最大直徑小於i毫米且平 123499.doc 200907139 均粒徑小於100微米。 本文所用術語”成膜”意指材料 在不存在其他試劑之情況下形成_連==合成條件下 本文所用術語,•非成膜,,意指材料在本文揭示之 下在不存在其他試劑之情況下不能形成—連續薄膜成條件 本文所用術语”織物"意指任何由纖維及/或紗線組合之 織、不織物、針織、栽絨、魅合、編織、或黏結材料200907139 IX. Description of the invention: [Technical field to which the invention pertains] Polyamine-based oximes having fabric care properties are included. The present invention also provides a knee-washing agent and a fabric softening agent, and a mouth softening agent, which comprises a polyamine <treatment group [Prior Art] A uremic urea-forming urea composition. == added to the detergent to impart a reduction in electrostatic adsorption, giving pleasure to... Less sensitive folds and easier to iron... Reduced ^, dried time, reduced - followed by time =. However, the benefit of these characteristics is usually that the == component is based on a long-chain fat called a quaternary compound = "quality is cationic. Therefore, it is soft to prevent the introduction of fabric during the period of substantially washable or dry = Looking at the reaction, usually in the fabric punching force = less time and cost of fabric washing county 'in the industry need to be compatible with the detergent composition. The industry also needs to be able to soften the fabric with the body The duration of the various benefits of ease of care and the use of an extended fabric care composition. [SUMMARY] The present invention provides a combination of a polyurethane-based fabric softener composition in the form of a powder or an aqueous dispersion. In a preferred embodiment, the fabric care composition is in the form of a nonionic film-forming dispersion comprising a polyaminocarbamic acid 123499.doc 200907139 urea polymer and water. The polymer prepolymer and the chain The reaction product of the water of the extender, wherein the prepolymer is a reaction of a mixture of a glycol or a plurality of diols with a polyisocyanate such as 4,4,-methylenebis(phenylisocyanate) Product. Another embodiment is a nonionic non-film-forming dispersion comprising water and a polyurethane urea polymer. The polymer is a reaction product of a prepolymer with a chain extender such as a diamine chain extender 'water and combinations thereof, wherein The prepolymer is a reaction product of a diol (polyol) or a mixture of a diol and a polyisocyanate (for example, 4,4,-methylenebis(n-iso-iso-acid). The polymer can then be converted. And grinding or spray drying to provide a powder. Yet another embodiment provides a method of extending the aroma or aroma of the fabric or garment. The method comprises contacting the fabric or garment with a scented oil and in the form of a powder or an aqueous dispersion. Polyurethane urea composition. The contacting can occur in a variety of ways including, but not limited to, the addition of sesame oil and polyurethane urea to a detergent or fabric softener prior to washing and/or drying the fabric. It is added directly to the wash water, or it is introduced directly or in combination with the fabric softener composition during the rinse cycle. Yet another embodiment provides a method of providing a desired property to a fabric or garment. This includes contacting the fabric with a polyurethane urethane in the form of a powder or an aqueous dispersion. The desired properties imparted to the fabric include, but are not limited to, shape retention, ease of care (i.e., easy ironing), and resistance to stationing. [Embodiment] The term "powder" as used herein means a particulate material composed of loose agglomerates of fine solid particles having a maximum diameter of less than i mm and a flat 123499.doc 200907139 average particle diameter of less than 100 μm. The term "film forming" as used herein means that the material is formed in the absence of other reagents. _ _ == The term used herein under synthetic conditions, • non-film forming, meaning that the material is not disclosed in the presence of other reagents. Conditions cannot be formed - continuous film forming conditions The term "fabric" as used herein means any woven, non-woven, knitted, tufted, fused, woven, or bonded material composed of fibers and/or yarn combinations.
包括(但不限於)彼等用於衣物(衣服)、被褥、毛巾、及: 簾者。 匈 本文所用術語”織物護理組合物”係指任何可應用於織物 (尤其在織物洗滌或乾燥期間)以賦予織物有益特性之 物。此等特性包括清潔、去除.、由、、t '' 月办云除油/貝及巧漬、使織物手减光 滑、減少靜電吸附、賦予令人愉悦之香氣、減少乾燥時 間、減少皺折且使熨燙更容易。 本文所提供之聚胺基甲酸_服組合物與目前市售織物護 理組合物相比提供令人f狀經改良織物形狀保持特性。 另外,其亦為織物提供易護理性或易於護理之特性。換言 之,經聚胺基甲酸酯脲組合物處理之織物洗滌後褶皺更少 且更易熨费。 某一些實施例之聚胺基甲酸酯脲亦具有令人驚訝之良好 水及油吸收(尤其當應用於織物時)。此對於抗污特性尤為 重要。織物與一些實施例之聚胺基甲酸酯脲組合物接觸 後,聚胺基甲酸酯脲將自污點造成源吸收濕氣及油且由此 限制織物本身對其之吸收。 I23499.doc 200907139 由於聚胺基甲酸酯脲組合物之吸收特性’其亦有助於延 長已與該組合物接觸之織物的香氣實體化。此係聚胺基甲 酸酯脲組合物對香油之吸收及隨後逐漸釋放之結果。 業内有一系列良好沈積或良好保持於聚胺基曱酸酯脲上 之香味材料。此等材料包括(但不限於)下列兩類A類及b 類’如下文所闡述者。 A類.羥基材料,其係辛醇/水分配係數(p)之常用對數 (l〇gi。P)係2.5或更咼、且氣體層析K〇vats指數(如針對聚二 甲基石夕氧烧作為非極性固定相所測定)至少為1〇5〇之醇、 苯紛或水揚酸酯。 在文獻中辛醇-水分配係數(或其常用對數"l〇gP")已作為 疏水性及水溶性之指示而為人們所熟知(參見11&11^11及1^0, Chemical Reviews,71,526_616,(1971); Hansch,(^以⑽及These include, but are not limited to, those used for clothing (clothing), bedding, towels, and curtains. Hungry The term "fabric care composition" as used herein refers to any article that can be applied to fabrics, especially during fabric washing or drying, to impart beneficial properties to the fabric. These features include cleaning, removal, and, t'' monthly cloud degreasing/shell and clever stains, smoothing fabric hands, reducing electrostatic adsorption, imparting pleasant aroma, reducing drying time, and reducing wrinkles And make ironing easier. The polycarbamic acid-coating compositions provided herein provide f-like improved fabric shape retention characteristics as compared to currently commercially available fabric care compositions. In addition, it also provides fabrics with ease of care or ease of care. In other words, the fabric treated with the polyurethaneurea composition has less wrinkles after washing and is easier to iron. The polyurethane urethanes of certain embodiments also have surprisingly good water and oil absorption (especially when applied to fabrics). This is especially important for stain resistance. After the fabric is contacted with the polyurethane urethane composition of some embodiments, the polyurethane urethane will absorb moisture and oil from the source of the stain and thereby limit the absorption of the fabric itself. I23499.doc 200907139 The absorption characteristics of the polyurethaneurea composition' also contribute to the elongation of the aroma of the fabric that has been in contact with the composition. This is the result of absorption and subsequent gradual release of the urethane composition from the urethane composition. There are a range of fragrance materials in the industry that are well deposited or well retained on the polyurethane uret urea. Such materials include, but are not limited to, the following two categories, Class A and Class B, as set forth below. Class A. Hydroxyl material, which is the common logarithm of the octanol/water partition coefficient (p) (l〇gi.P) is 2.5 or more, and the gas chromatographic K〇vats index (eg for polydimethyl sch Oxygen is determined as a non-polar stationary phase) of at least 1 〇 5 〇 of alcohol, benzene or salicylate. The octanol-water partition coefficient (or its usual logarithm "l〇gP") has been well known in the literature as an indicator of hydrophobicity and water solubility (see 11 & 11^11 and 1^0, Chemical Reviews, 71, 526_616, (1971); Hansch, (^ with (10) and
Lawrence, J. Organic Chemistry, 33,347-350 (1968))。當 此專值無法自文獻中得到時’其可直接量測,或使用數學 算法大致估計。提供此等估計之軟體可自市場購得,例如 得自 Advanced Chemistry Design公司之,’LogP"。 logio P為2.5或更高之材料具有相當疏水性。Lawrence, J. Organic Chemistry, 33, 347-350 (1968)). When this value cannot be obtained from the literature, it can be measured directly or roughly estimated using a mathematical algorithm. Software providing such estimates is commercially available, for example, from Advanced Chemistry Design, 'LogP". Materials with a logio P of 2.5 or higher are quite hydrophobic.
Kovats指數係根據在氣體層析量測中之保留時間參照烷 烴之保留時間來計算[參見K〇vats, Helv. Chim. Acta 41, 1915 (1958)]。在香油業内將基於使用非極性固定相之指 數香油作為組份分子大小及沸點之描述符已達若干年。香 油業中Kovats指數之闡述由τ Shibamoto於,'Capillary GasThe Kovats index is calculated based on the retention time of the alkane based on the retention time in gas chromatography measurements [see K〇vats, Helv. Chim. Acta 41, 1915 (1958)]. In the sesame oil industry, the index based on the use of non-polar stationary phase fragrant oil has been used as a descriptor for the molecular size and boiling point of the component for several years. The description of the Kovats index in the sesame industry by τ Shibamoto, 'Capillary Gas
Chromatography in Essential Oil Analysis", p Sandra及 C 123499.doc 200907139Chromatography in Essential Oil Analysis", p Sandra and C 123499.doc 200907139
Bicchi(編輯)’ Huethig (1987),第 259-274頁中給出。適合 之普通非極性相係100%二甲基聚矽氧烷,如以(例如)多種 商品名(例如RP-1 (Hewlett-Packard)、cp Sil 5 CB(Chrompack)、 〇V-l(〇hio Valley)及 Rtx-l(Restek))所提供者。 低Kovats指數材料易於揮發且在許多織物上不能良好保 持。 A類包括具有通式R〇H之醇,其中該經基可係一級、二 級或二級經基,並且該R基團係一視情況具支鏈或經取 代、環狀或非環狀之烷基或烯基,以使R0H具有上述所定 義之分配係數及Kovats特性。Kovats指數介於1050至1 600 之醇通常係分子量介於150至230間之單官能團烷基或芳基 烧基醇。 A類亦包括具有通式Ar〇H之酚,其中該Ar基團代表可經 一或多個烷基或烯基 '或經基團_C〇2A(其中A係一烴基團) 之酷(在此情況下該化合物係水揚酸酯)取代的苯環。Ar〇Ii 具有如上所定義之分配係數及K〇vats指數。通常,此等 Kovats係數為1〇50至16〇〇之酚係分子量在15〇至21〇範圍内 之單羥基酚。 A類香油材料之實例係1-(2,-第三-丁基環己氧基)_ 丁 _2_ 醇、3-甲基-5-(2,,2|,3’_三甲基環戊_3_烯基)_戊_2_醇、4_甲 基-3-癸烯_5_醇、水楊酸戊酯、2_乙基_4_(2,,2,,3_三甲基環 戊3稀基)丁-2 -歸醇、莰醇、香芹酴、香茅醇、9_癸稀 醇、二氫丁香酚、二氫裏哪醇(dihydrolinalol)、二氫月桂 烯醇、二氫松油醇、丁香酚、香葉醇、羥基香茅醛、水揚 123499.doc 200907139 酸異戊酯、水揚酸里 ,,.. "知 '異丁香酚、裏哪醇、薄荷醇、 橙花三級醇、橙花 對第二-丁基環己醇、苯氧基乙 酉予喊烯醇、四氫香荦醅 斤 m ^ ν ” %、四虱裏哪醇、四氫月桂烯醇、 麝香卓紛、2_甲氧基μ f基酚、(4-異丙基環己基)_甲醇、 水揚酸苄基酯、水楊酸 ^ 衣己基g日、水楊酸己酯、廣藿香 醇、及金合歡醇。 ’、 B類:S旨、醚、暗、;^上、 ^ 鲷或醛,其辛醇/水分配係數(P)之 吊用對數值(l〇g1〇 p)為2 s ·+、s ^ )马2.5或更咼,且氣體層析K〇vats指數 (如針對聚二甲基矽氧俨 /巩烷作為非極性固定相所測定 為 1300 〇 B類香油係具有通戎 一 者’,、中X可處於一級、二級或Bicchi (ed.) Huetig (1987), pp. 259-274. Suitable for the general non-polar phase system 100% dimethyl polyoxane, for example, under various trade names (eg RP-1 (Hewlett-Packard), cp Sil 5 CB (Chrompack), 〇Vl (〇hio Valley) ) and Rtx-l (Restek)). Low Kovats index materials are volatile and do not hold well on many fabrics. Class A includes alcohols having the formula R〇H, wherein the thiol group can be a primary, secondary or secondary transradical, and the R group is optionally branched or substituted, cyclic or acyclic. An alkyl or alkenyl group such that ROH has the partition coefficient and Kovats properties as defined above. The alcohol having a Kovats index of from 1050 to 1 600 is usually a monofunctional alkyl or aryl alkyl alcohol having a molecular weight of from 150 to 230. Class A also includes phenols of the formula Ar〇H, wherein the Ar group represents a bond which may be via one or more alkyl or alkenyl groups or via a group _C〇2A (wherein A is a hydrocarbon group) In this case the compound is a salicylate substituted benzene ring. Ar〇Ii has a partition coefficient as defined above and a K〇vats index. Usually, these Kovats coefficients are from 1 to 50 to 16 Å of phenolic monohydric phenol having a molecular weight in the range of 15 Å to 21 Å. An example of a class A sesame oil material is 1-(2,-tri-butylcyclohexyloxy)-butan-2-ol, 3-methyl-5-(2,,2|,3'-trimethylcyclo Pentyl-3-enyl)-pent-2-ol, 4-methyl-3-decene-5-alcohol, amyl salicylate, 2_ethyl_4_(2,,2,,3_3 Methylcyclopentazenyl)butane-2 -homyl alcohol, decyl alcohol, carnation, citronellol, 9-decane, dihydroeugenol, dihydrolinalol, dihydromyrcene Alcohol, dihydroterpineol, eugenol, geraniol, hydroxycitronellal, shuiyang 123499.doc 200907139 isovalerate, salicylic acid, .. " knowing 'isoeugenol, linalool , menthol, nerolitriol, neroli to di-butylcyclohexanol, phenoxyethyl hydrazine, ethenyl alcohol, tetrahydro citron, m ^ ν ” %, tetralinol, four Hydrogen lauryl alcohol, musk, 2_methoxy μf-based phenol, (4-isopropylcyclohexyl)-methanol, benzyl salicylate, salicylic acid, hexyl group, salicylic acid Hexyl ester, patchouli alcohol, and farnesol. ', Class B: S, ether, dark, ^^, ^ 鲷 or aldehyde, its octanol/water partition coefficient (P) hanging logarithm (l〇g1〇p) is 2 s ·+, s ^ ) horse 2.5 or more, and the gas chromatographic K〇vats index (eg for polydimethyl hydrazine/contained as a non-polar stationary phase) For the 1300 〇B type scented oil system has one wanted one, and the middle X can be in the first, second or
三級位,並且係下列之群中之一 :_c〇2A、儒、KN 或-CHO。基團!^及A係環狀或非環狀且視情況經取代之煙 殘基。通常,K〇vats指數不超過16〇〇之_ 介於16〇至230之間之單官能團化合物。 B類香油材料之實例车 J係1-甲基-4-(4-甲基戊烯基)_3_環 己稀小甲酸、Η,二甲基環己烯基)_戊-稀小酮、2_庚 基環戊酮、2_甲基_3-(4,_第三-丁基苯基)丙駿、2_甲基十一 酸、2_十一稀駿、2,2~二甲基邻,-乙基苯基^酸、 3-(4’-異丙基苯基)·2_甲基丙酸、乙酸”基_4_苯基戊_2_ 基醋、環己基丙酸稀丙基醋、環己氧基乙酸烯丙基醋、苯 甲酸戍Sl、甲基乙基蜩三聚體、二苯甲ig、3·(4,.第三-丁 基本基)-丙酸、丁香婦、順式·茉莉酮、擰檬駿二乙基乙縮 醛、香茅醛二乙基乙縮醛、乙酸香茅酯、苯基乙基丁基 I23499.doc 200907139 醚、α-大馬酮、β-大馬酮、δ-大馬酮、γ_大馬酮、二氫異 茉莉酮酸酯、二氫茉莉S同、乙酸二氫萜品酯、鄰胺基苯甲 酸二甲酯、二苯醚、一苯基甲烷、十二醛、十二烯_2•醛、 十二腈、1-乙氧基-1-苯氧基乙烷、3 _(Γ_乙氧基乙氧 基)-3,7-二曱基辛-1,6-二烯、4·(4,_甲基戊_3,_烯基)_環己-3_ 烯醛、三環[5.2.1.〇-2,6-]癸烷_2_曱酸乙酯、1-(7_異丙基_5_ 曱基雙環[2.2.2]辛-5-烯-2-基)_卜乙酮、烯丙基三環癸烯 醚、丙酸三環癸烯基酯、γ、十一烷酸内酯、正曱基正苯 基-2-曱基丁醯胺、異丁酸三環癸烯酯、乙酸香葉酯、苯甲 酸己酯、紫羅酮α、紫羅S同β、肉桂酸異丁酯、異丁基喹 啉、乙酸異丁香酯、2,2,7,7-四甲基三環十一 _5_酮、乙酸 三環癸烯基酯、2-己基環戊酮、4-乙醯氧基_3_戊基四氫吡 喃、2-己基乙醯乙酸乙酯、8-異丙基_6_曱基雙環[2 2.2] 辛-5-烯-2-甲醛、4-異丙基-1_甲基雙環[2.2.2]辛_5_烯_2_甲 酸曱酯、肉桂酸甲酯、α異甲基紫羅酮、曱基萘基酮、橙 花醚、壬内酯γ、乙酸壬酯、乙酸對第三-丁基環己基酯、 4-異丙基-1-曱基-2-[1·-丙烯基]-苯、異丁酸苯氧基乙酯、 苯基乙基異戊醚、異丁酸苯基乙酯、新戊酸三環癸烯酯、 新戊酸苯基乙酯、苯乙醛乙二醇縮醛、2,4_二甲基_4_苯基 四虱吱°南、玫瑰丙酮、乙酸萜品酿、4 -異丙基_1_甲基_2_ [1'-丙烯基]、苯、2-萘甲醚、甲酸(4-異丙基環己二烯基)乙 醋、肉桂酸戊酯、戊基肉桂醛、戊基肉桂醛二甲基縮醛、 肉桂酸肉桂酯、1,2,3,5,6,7,8,8&_八氫_1,2,8,8_四甲基_2_乙 醒基奈、環-1,13 -伸乙基二氧基三癸_1,13 -二酮、環十五内 123499.doc -32- 200907139 6曰己基肉桂酸、1,3,4,6,7,8-六氫_4,6,6,7,8,8_六甲基環戍 [g] 2苯#比南、苯乙酸香葉酯、&乙醯基小異丙 基-2,3,3,5-四甲基二氳節、及u,2,4,4,7_六曱基胃6乙醯 基·1,2,3,4-四氫萘。 儘管此係與氨綸組合物-起作用尤為良好之香油及香料 的廣泛列纟,但應認識到多種其他香油亦可用於一此實施 卩中茲香油可包括—種物質或物質混合物,其包括天然 (即,藉由花、草、葉、樜…丄 物獲得者卜人、、树皮、木材、花或植物提取 (不同天然油或油成分混合物)及合成 (即,以合成方式產生者)氣味物質。 可用香油之非限制性列表 醛;;m Μ 1 表I括.己基肉桂醛;戊基肉桂 水楊酸戊酯;水棍舻 . 式_2 次己Sa ;萜品醇;3,7-二曱基-順 ' 2,6-辛二烯 _;!_ 醇;2,6-二 T 基"2 ·辛 Sj· ? 2,6 · 一 审其 i jL· 烯_2·醇;3,7-二甲基_3 ^ ,6 —甲基_7_辛 烯i π 辛醇;3,7_二甲基·反式-2,6-辛二 烯-1-醇;3,7_二甲基 ’ ψ A , r 中席酉予,3,7_二甲基-1-辛醇;2_ T基-3-(對-第三-丁基 ^ X . 土)-丙醃;4_(4_羥基-4_甲基戊 基己烯-1-甲醛._ 一 s 戊 W巷砍。酸二環癸烯醋;乙酸三環癸烯 日’回香醛;2-甲基_2_(對_里 . ; 3-f ^-3- …:“基酿;4_(對_經基苯基)_ (A6,6-三甲基·2_頊 ^ Γ , -土)-2- 丁烯·1-顚I丨對-甲氧其 本乙_,·對_甲氧基 對甲氧基 酸甲酯.+ m t 歸正己基·3_氧代·環戊烷羧 〒西曰,十一内酯γ、橙油 油;丁香油.十…t 才豕油,柚子油;香檸檬 甲基『γ;2_(2-戊基·3·氧代-環戊基)乙酸 r丞酉曰,β_萘酚甲 甲基-β-萘基酮;香豆素;癸醛;苯 123499.doc -13- 200907139 曱路,乙酸4-第三-丁基環己基酯;乙酸α,α-二甲基苯乙基 酉曰’乙酸曱基苯基原酯;十三烧二酸之環狀乙二醇二酯; 3,7_二甲基-2,6-辛二烯-i-腈;紫羅酮γ甲基;紫羅酮α ;紫 羅嗣Ρ,卑檸油;甲基柏木酮;7-乙醯基_1,2,3,4,5,6,7,8-八Tertiary, and one of the following groups: _c〇2A, Confucian, KN or -CHO. Group! ^ and A are cyclic or acyclic and optionally substituted tobacco residues. Typically, the K〇vats index does not exceed 16 单 between 16〇 and 230 monofunctional compounds. An example of a B-type scented oil material is J-based 1-methyl-4-(4-methylpentenyl)_3_cyclohexene small formic acid, hydrazine, dimethylcyclohexenyl) pentane-dione 2_heptylcyclopentanone, 2_methyl_3-(4,_t-butylphenyl)propyl, 2-methylundecanoic acid, 2_11 稀, 2,2~2 Methyl o-, -ethylphenyl-acid, 3-(4'-isopropylphenyl)-2-methylpropionic acid, acetic acid"-based 4-phenylpentan-2-yl vinegar, cyclohexylpropionic acid Dilyl propyl vinegar, cyclohexyloxyacetic acid allyl vinegar, bismuth benzoate s, methyl ethyl hydrazine trimer, diphenyl ig, 3 (4,. tri-butyl phenyl)-propionic acid , lavender, cis-jasmone, spirulina diethyl acetal, citronellal diethyl acetal, citronellyl acetate, phenylethylbutyl I23499.doc 200907139 ether, α-large Ketone, β-Damarone, δ-Damascone, γ_Damasolone, Dihydroisojasmonate, Dihydro Jasmine S, Dihydrofurfuryl acetate, Dimethyl ortho-benzoate , diphenyl ether, monophenylmethane, dodecanal, dodecene _2 aldehyde, dodecanenitrile, 1-ethoxy-1-phenoxyethane, 3 _(Γ_ethoxy ethoxylate Base)-3,7-dimercapto-1 6-diene, 4·(4,_methylpenta-3,-alkenyl)-cyclohex-3-enal, tricyclo[5.2.1.〇-2,6-]decane_2_decanoic acid Ethyl ester, 1-(7-isopropyl-5-nonylbicyclo[2.2.2]oct-5-en-2-yl)-e-ketone, allyl tricyclodecene ether, tricyclic guanidinium propionate Alkenyl ester, γ, undecanoic acid lactone, n-decyl-n-phenyl-2-mercaptobutylamine, tricyclodecenyl isobutyrate, geranyl acetate, hexyl benzoate, ionone α, violet S with β, isobutyl cinnamate, isobutylquinoline, iso-syringyl acetate, 2,2,7,7-tetramethyltricyclo eleven-5-one, tricyclodecene acetate Base ester, 2-hexylcyclopentanone, 4-ethenyloxy_3_pentyltetrahydropyran, ethyl 2-hexylacetate, 8-isopropyl-6-indenylbicyclo[2 2.2] Oct-5-ene-2-carbaldehyde, 4-isopropyl-1-methylbicyclo[2.2.2]oct-5-ene-2-carboxylic acid decyl ester, methyl cinnamate, alpha isomethylionone , decylnaphthyl ketone, neroli, azlactone γ, decyl acetate, acetic acid to tert-butylcyclohexyl ester, 4-isopropyl-1-indenyl-2-[1·-propenyl ]-Benzene, phenoxyethyl isobutyrate, phenylethyl isoamyl ether, phenylethyl isobutyrate, pivalic acid Terpene ester, phenylethyl pivalate, phenylacetaldehyde glycol acetal, 2,4-dimethyl-4-ylphenyltetradecyl, rose acetone, acetic acid, 4 - different Propyl_1_methyl_2_[1'-propenyl], benzene, 2-naphthylmethyl ether, (4-isopropylcyclohexadienyl) formate, pentyl cinnamate, amyl cinnamaldehyde , amyl cinnamaldehyde dimethyl acetal, cinnamic cinnamate, 1,2,3,5,6,7,8,8&_octahydro-1,2,8,8-tetramethyl_2_ Ethyl ketone, ring-1,13-extended ethyldioxytrisulphate_1,13-dione, ring fifteen inside 123499.doc -32- 200907139 6 hexyl cinnamic acid, 1,3,4, 6,7,8-hexahydro_4,6,6,7,8,8-hexamethylcyclononanthene [g] 2 benzene #比南, phenylacetate geranyl ester, ðinyl isopropyl -2,3,3,5-tetramethyl diterpene, and u, 2,4,4,7_hexainyl 6-ethoxyl-1,2,3,4-tetrahydronaphthalene. Although this is in general agreement with spandex compositions - particularly good sesame oils and fragrances, it should be recognized that a variety of other sesame oils may also be used in this practice. The scented oil may include a substance or mixture of substances, including natural (ie, by flower, grass, leaf, cockroach... cockroach, bark, wood, flower or plant extract (mixture of different natural oils or oil components) and synthesis (ie, synthetically produced) Odor substance. A non-limiting list of emulsifiable aldehydes; m Μ 1 Table I includes hexyl cinnamaldehyde; amyl cinnamate salicylate; water stick 舻. _2 己 Sa Sa; terpineol; 7-dimercapto-cis' 2,6-octadiene _;!_ alcohol; 2,6-di-T base"2 · 辛Sj· ? 2,6 · first trial of its i jL·ene-2·alcohol 3,7-Dimethyl_3^,6-methyl-7-octene i π octanol; 3,7-dimethyl-trans-2,6-octadien-1-ol; , 7_ dimethyl ' ψ A , r 酉 酉 , 3,7-dimethyl-1-octanol; 2_ T-based-3-(p-tri-butyl ^ X. soil)-acrylic; 4_(4_hydroxy-4_methylpentylhexene-1-carbaldehyde._ a s pentyl W lane cut. Acid bicyclic terpene vinegar; acetic acid Cyclodecene ' 回 aldehyde; 2-methyl 2 _ (p-_ _. 3-f ^ -3- ...: "base brew; 4 _ (p- phenyl) phenyl) (A6, 6-three Methyl·2_顼^ Γ , -土)-2-butene·1-顚I丨--methoxybenzamine B,·p-methoxy-p-methoxy acid methyl ester.+ mt 3·oxo·cyclopentane carboxy oxime, eleven lactone γ, orange oil; clove oil. Ten...t 豕 oil, grapefruit oil; bergamot methyl γ; 2_(2-penta ··3·oxo-cyclopentyl)acetic acid r丞酉曰, β-naphtholmethylmethyl-β-naphthyl ketone; coumarin; furfural; benzene 123499.doc -13- 200907139 曱路, acetic acid 4-tert-butylcyclohexyl ester; α,α-dimethylphenethyl hydrazide acetate decyl phenyl orthoester; cyclic ethylene glycol diester of thirteen succinic acid; 3,7 _ dimethyl-2,6-octadiene-i-nitrile; ionone γ methyl; ionone α; sorghum, sulphur oil; methyl cedarone; 7-ethenyl_1 , 2,3,4,5,6,7,8-eight
氫-1,1,6,7·四曱基-萘;紫羅酮曱基;甲基-1,6,1〇-三甲 基_2,5,9-環十二烧三烯-1-基酮;7-乙醯基-I,1,3,4,4,6-六曱 基四氫萘;4·乙醯基-6-第三-丁基-1,1-二甲基二氫茚;二 苯甲酮;6-乙醯基^山^弘六曱基二氫茚:^乙醯基冬 異丙基-1,1,2,6-四曱基二氫茚;卜十二醛;7_羥基_3,7_二 曱基辛醛;1〇-十一烯_1-醛;異-己烯基環己基甲醛;甲醯 基二壞癸燒;環十五内酯;16_羥基_9_十六烯酸内酯; 1,3,4,6,7,8-六氫_4,6,6,7,8,8_六甲基環戊_7_2_苯并吡喃4; 龍涎香烷;十二氫_3a,6,6,9a_四曱基萘並_[2,lb]呋喃;雪 权.,5-(2,2,3-二甲基環戊_3_烯>3_甲基戊烷_2_醇;2_乙 基4 (2,2,3 —甲基_3_環戊稀小基)_2_ 丁烯小醇·,丁香烯 醇,乙酸柏木g旨;乙酿斜# — 己®夂對-第二-丁基環己基酯;廣霍香; 乳香松香脂;勞丹脂;巷#、, 香根卓油;古巴香脂;樅香脂;羥 基香茅越及°引ν朵;|其7„ _ 土乙路及吲哚;香葉醇;乙酸香葉 @旨,晨哪醇;乙酸裏哪酷.m斤* ^ 自日,四虱裏哪醇;香茅醇;乙酸香 茅酯,二氫月桂烯醇; ^ ®夂一虱月桂烯酯;四氫月桂烯 醇,乙酸φΙ品g旨;諾萄妒.7 ^ 泛動®子,乙酸諾蔔醇酯;2_苯基乙醇; 乙酸2 -苯基乙醋;苄醇.7缺— ^ ’乙酸卞酯;水楊酸苄酯;苯曱酸 苄酯;乙酸蘇合香酯;二 A , ^ 基基甲醇;甲基苯基三級甲 基乙酉夂二氯甲基苯基原酯. ,乙S久異壬酯;乙酸香根酯;香 J23499.doc •14- 200907139 根醇’ 2_甲基_3_(對-第三-丁基苯基)-丙酸;2-甲基-3-(對· 異丙基苯基)丙醛;3_(對-第三-丁基苯基)-丙醛;4*甲 基3戊烯基)_3_環己烯甲醛㈠-乙醯氧基戊基四氫哌 喃^二氫茉莉酉同酸甲商旨;2_正庚基環戍_ ; 3-甲基_2_戊 基%戊酮,正癸酸;正十二駿;9_癸婦醇七異丁酸苯氧 基乙基醋;苯乙醛二甲基縮醛;苯乙醛二乙基縮醛,·香葉 腈:香茅腈;柏木基縮醛;3_異莰基環己醇丨柏木基甲基 ^ 長葉烧嗣’回香腈;茴香駿;胡椒酸;丁香齡;香 草酸 H赵基香茅駿紫羅酮;f基紫羅酮;異甲基 紫羅if ;鳶尾酮;;値彳 順式-3-己烯醇及其酯;二氫茚麝香香 油;四氫萘麝香香油;異二氫苯并d比喃麝香香油;大環 酮;大環内醋麝香香油;巴西酸乙二醋,及其組合。 一些實施例之聚胺基甲酿_ Ββ g , t ,、 j T酸^脲可呈水性分散液或粉末形 式。當期望粉末形式時,1 ” 了藉由過濾、乾燥及研磨或藉 由复霧乾燥分散液自水性分埒 Η生刀放液分離出。就成膜或非成膜 液而言’分散液之固體含量係可變化的。舉例而言, 固體含量可為約5%至約50%,苴包 八栝刀散液的約2〇重量 至約4 0重量%、及分今、、右ώ 放液自、.々32重量。/。至約37重量%。 分散液黏度亦可根攄用# ^m 途而有所不同。適合之黏度實例 =括自約4叩至約36cps,包括自約8,至約IN。杂 :將分散液添加至諸如洗務劑或織物軟: 合物中時’期望其具有與織物護理組合物相似之:;、 分散液PH亦可根據其用途而有 - 於其中之織物護理組合物為酸性時,該田放液欲添加 刀政液之pH應係中 123499.doc -15- 200907139 性至酸性且期望其具有一類似於織物護理組合物之pH,其 包括pH 7或更低,例如pH 2-4。 為製備一些實施例之陰離子成膜水性分散液,需製備為 封端二醇之預聚物。適合預聚物之實例係如下之反應產 物: 至少一羥基端聚合物,例如聚醚(包括共聚醚)、聚碳酸 酯或一數量平均分子量為約600至約3,5〇〇之聚酯多元醇組 份,舉例而言,數量平均分子量為約^400至約2 4〇〇之聚 (四亞甲基醚)二醇; 多異氰酸酯,其係4,4,-及2,4,-亞曱基雙(苯基異氰酸 S曰)(MDI)異構體之混合物,其中異構 體之比率自約65:35至約35:65 ;及 至少一個具有下列基團之二醇化合物:⑴能與多異氰酸 酯之MDI異構體混合物反應之羥基及(ii)至少一個中和時能 形成鹽之羧酸基團,其中該至少一個羧酸基團不能與多異 氰酸醋之MDI異構體混合物反應。 然後藉由(例如)包含三乙胺來中和該預聚物以形成一鹽 並且最後使用二胺鏈延長劑及水進行鏈延長以形成水性分 散液。可包括諸如表面活性劑、防泡劑/消泡劑、抗氧化 劑、增稠劑及其組合等添加劑。 用於陰離子分散液之MDI異構體混合物不需添加溶劑即 可達成預聚物黏度之降低。MDI異構體混合物亦用於降低 反應速率。預聚物可經由間歇製程或連續製程來製備。 當二醇包括於一些實施例中時,可將包括羥基及羧酸基 123499.doc 16 200907139 團之一醇描述為酸性二醇。可用酸性二醇之實例包括2,2 -二經甲基乙酸、2,2-二羥甲基丙酸(]:)1^1>八)、2,2-二羥曱基 丁酸、2,2-一經甲基戊酸、及其組合。 —些實施例之非離子成膜分散液包括一為異氰酸酯端基 聚胺基甲酸酯預聚物之預聚物。適合預聚物之實例係羥基 J而基聚合物(例如多元醇’諸如聚(四亞甲基-共_伸乙基醚) —醇或聚(四亞甲基醚)二醇與乙氧基化聚丙二醇之混合物) 與二異氰酸酯(例如4,4,-亞甲基雙(苯基異氰酸酯))之反應 產物。隨後用水將該預聚物鏈延長並於水中分散或者分散 於水中之後用水將鏈延長。 一些實施例之非離子非成膜分散液包括係一異氰酸酯端 基聚胺基甲酸醋預聚物之預聚物。該預聚物亦係多元醇 (例如聚丁二烯二醇或聚(四亞甲基醚)二醇)與二異氰酸酯 (諸如4,亞甲基雙(苯基異氰酸醋))的反應產物。該預聚 物可使用水與二胺鍵延長劑(例如乙二胺或諸如聚乙稀胺 等胺-官能團交聯劑)之組合進行鏈延長。可選擇一親水或 疏水二醇以生產一具有不同水/油吸收能力之聚合物粉 末。另外’粉末粒控可藉由借助於稀釋溶劑調節預聚物黏 η ^ Ί7'4 ^ ν 诉〜π —哔 < 預聚物,將 4散至水中以使鏈延長。為製備此等分散液,可將水冷 部以在鏈延長反應開始之前更完全分散。舉例…可: 至約""Μ低,包括約7°C或更低。多種來源之 ”些實例之为散液-起使用,例如蒸顧水、去離子 l23499.d〇c • 17- 200907139 水或超純水。 對於非成膜或成膜分散液而言,分散液中粒子之平均粒 控均係可變化的。如上文所述’影響粒徑之一因素係預聚 物之黏度。另一因素係分散速度,其可為(例如)約5,〇〇〇 rpm至約l〇,〇〇〇 rpm ’包括7,〇0〇 rpm。一些實施例之分散 液及粉末的粒徑範圍包括約400微米(μιη)或更小,例如約 0.01 μπι至约 0.5 μηι、0.1 μηι至約 1.0 μηι、約 01 μηι至約 5 〇 μιη、約〇·15 μιη至約0.65 μιη、及更大粒子(例如自約1〇 μιη 至約 1 5 0 μηι)。 在一些實施例中,聚胺基曱酸酯脲粉末係藉由在有或沒 有溶劑之情況下將異氰酸酯端基預聚物高剪切力分散至含 有分散劑、及鏈延長劑或交聯劑之水介質中來製備。高剪 切力定義為足以使粒子不大於5〇〇微米之力。該預聚物可 藉由多元醇或多元醇共聚物或多元醇混合物(例如聚醚二 醇、聚酯二醇、聚碳酸酯二醇、聚丁二烯二醇或其氫化衍 生物、及冑基端基聚二曱基石夕氧院)與〕異氰酸酿(諸如亞 甲基雙(4-苯基異氰酸酯)(MDI))反應以形成nc〇_端基預聚 物或'’封端二醇"來製備。在聚合物組合物中,NCO/〇H之 莫耳比率係”於1.2至5.〇之間。鏈延長試劑之實例係脂肪 族二胺,例如乙二胺(EDA)。 當期望粉末交聯時,鏈交聯劑可係—至少具有三個能與 腳基團反應之―級胺或二劑胺官能團之有機化合物或聚 合物。 溶解或不〉谷於水中之右撼C交添丨,y 甲之有機/合劑(例如1_甲基2-咄咯啶酮 123499.doc -18- 200907139 (NMP)或二甲苯)可用於在分散前稀釋預聚物。分散於水中 之所形成聚胺基甲酸醋脲聚合物細粒可如此使用或藉由過 據及乾燥分離成固體粉末。或者,亦可使用一亦提供更高 粒徑控制之喷塗製程。 一些實施狀Μ粒徑可根據其期望賴而改變。舉例 而言,平均粒徑可小於1毫米(峨),#包括小於⑽微米 (μιη)之平均粒徑。 在-些實施例中’用於製備彈性體粉末之礙段聚胺基甲 酸醋脲包括:a)數量平均分子量介於500至5_之多元醇 或多元醇共聚物或多元醇屍合物,其包括但不限於聚t 醇、聚醋二醇、聚碳酸賴二醇、聚丁二婦二醇或其氯化衍 生物、及备基端基聚二甲基石夕氧烧;b)二異氛酸醋,盆包 t脂肪族二異氰酸醋、芳族二異氰酸醋、環脂族二異氰酸 s曰,及c)脂肪族二胺(gp,_ (卩一胺鏈延長劑)或其與至少一個 選自由脂肪族二胺及環脂族二 胺G、各具有2至13個碳原子) ::成之群之二胺的混合物 '或胺基端基聚合物、或具有至 V 一個一級或二級胺基團之有機彳b入物4 圓之有機化合物或聚合物;及視情 '、及或—級單胺作為鏈終止劑。 可用於某此眘谂A,丨—& 個…多元醇之實例包括彼等具有兩 個或兩個以上翔其 ^ ^ 焱基之—知,其自環氧乙 雜環丁烷、四舒岵咗π 衣氧丙烷、氧 風夫南、及3_尹基四氫咬唾經由開環聚合反 應及/或共聚獲得,或自多㈣⑽如,每 於12個碳原刀于Τ具有) iq/丁 醇或二醇混合物,例如乙二醇、丙 ,丁二醇、丨,5-戍二醇、己二醇、新戍二醇、 123499.doc -19· 200907139 3-甲基-1,5-戊二醇、1,7-庚二醇' 1,8_辛二醇、1;9_壬二 醇、1,10 -癸一醇及1,12 -十一烧一醇)經縮聚獲得。舉例而 言,可包括一直鏈、雙官能團聚醚多元醇,尤其分子量為 約1700至2100之聚(四亞曱基朗1)二醇,例如官能度為2之Hydrogen-1,1,6,7·tetradecyl-naphthalene; ionone oxime; methyl-1,6,1〇-trimethyl-2,5,9-cyclododecatriene-1 -ketone; 7-ethenyl-I,1,3,4,4,6-hexamethylenetetrahydronaphthalene; 4·ethinyl-6-tri-butyl-1,1-dimethyl Dihydroanthracene; benzophenone; 6-ethyl fluorenyl group; mountain 弘 曱 曱 曱 二 dihydro hydrazine: ^ ethoxylated isopropyl-1,1,2,6-tetradecyldihydroanthracene; Dodecanal; 7-hydroxy-3,7-didecyloctanoyl; 1〇-undecene-1-aldehyde; iso-hexenylcyclohexylcarbaldehyde; formazan-based gangrene; Ester; 16_hydroxy_9_hexadecenolactone; 1,3,4,6,7,8-hexahydro_4,6,6,7,8,8-hexamethylcyclopentyl_7_2_ Benzopyran 4; ammonium; dodecaine_3a,6,6,9a_tetradecylnaphthalene-[2,lb]furan; Xuequan.,5-(2,2,3-two Methylcyclopenta-3-ene >3_methylpentane-2-ol; 2_ethyl 4 (2,2,3-methyl_3_cyclopentanyl)_2_butenol , syringenol, acetaminophen acetate; B-branched #— hexyl-p-butyl-butylcyclohexyl ester; Guanghuoxiang; frankincense rosin; labdanum; lane #,, fragrant oil; Cuba Balsam; eucalyptus; hydroxy citronella and ° quot ;|其七„ _ 土乙路 and 吲哚; geraniol; acetic acid fragrant leaves @旨, Chennaol; acetic acid which cool. m kg * ^ from the day, tetraterpene alcohol; citronellol; acetic acid Citronellol, dihydromyrcenol; ^ ® 夂 虱 虱 烯 ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; Phenylethanol; 2-phenylethyl acetate; benzyl alcohol. 7 deficiency - ^ 'Oxyl acetate; benzyl salicylate; benzyl benzoate; sulphate acetate; di A, ^ benzyl methanol; Phenyl tertiary methyl ethyl hydrazine dichloromethyl phenyl orthoester. , Ethyl sulphate; Acetyl acetate; Fragrance J23499.doc • 14- 200907139 Root alcohol ' 2 _ _ 3_ (for - Tert-butylphenyl)-propionic acid; 2-methyl-3-(p-isopropyl)phenylpropanal; 3-(p-tris-butylphenyl)-propanal; 4*A 3-pentenyl)_3_cyclohexenecarbaldehyde (I)-acetoxypentyltetrahydropyran^dihydrojasmine oxime acid; 2_n-heptylcycloindole _ ; 3-methyl_2 _Pentyl% pentanone, n-decanoic acid; Zheng 12; 9_chewing alcohol hexaisobutyric acid phenoxyethyl vine; phenylacetaldehyde dimethyl acetal; phenylacetaldehyde Ethyl acetal, geranyl nitrile: citronellin; cedar acetal; 3_isodecylcyclohexanol cedaryl methyl ^ long leaf simmered 回 回 carbonitrile; fennel; pepper acid; ; vanillic acid H Zhaojixiang Maojun ionone; f-based ionone; isomethyl violet if; ketone; 値彳 cis-3-hexenol and its ester; dihydro eucalyptus oil; tetrahydrogen Naphthoquinone scented oil; iso-dihydrobenzo-d-pyrene sesame oil; macrocyclic ketone; macrocyclic vinegar eucalyptus oil; brazil acid vinegar, and combinations thereof. The polyaminoglycines _ Ββ g , t , , j T acid urea of some embodiments may be in the form of an aqueous dispersion or powder. When a powder form is desired, 1" is separated from the aqueous bifurcated knife by filtration, drying and grinding or by a re-drying dispersion. For a film-forming or non-film-forming liquid, 'dispersion The solid content may vary. For example, the solid content may be from about 5% to about 50%, from about 2 ounces to about 40% by weight of the balsam pebbles, and the right, right, and right The liquid is from 32% by weight to about 37% by weight. The viscosity of the dispersion may also vary depending on the way. The viscosity example is suitable from about 4 叩 to about 36 cps, including self-approximately. 8. To about IN. Miscellaneous: When the dispersion is added to, for example, a detergent or a soft fabric, it is expected to have a similar texture to the fabric care composition:; the dispersion PH may also be used depending on its use - Where the fabric care composition is acidic, the pH of the field liquid to be added to the knife solution is 123499.doc -15-200907139 to acidic and it is expected to have a pH similar to the fabric care composition, Including pH 7 or lower, such as pH 2-4. To prepare an anionic film-forming aqueous dispersion of some embodiments, preparation is required. Prepolymers of blocked diols. Examples of suitable prepolymers are the following reaction products: at least one hydroxyl terminated polymer, such as a polyether (including copolyether), polycarbonate or a number average molecular weight of from about 600 to about a polyester polyol component of 3,5 Å, for example, a poly(tetramethylene ether) diol having a number average molecular weight of from about 400 to about 24 Å; a polyisocyanate of 4, 4 a mixture of -, and 2,4,-arylene-bis(phenylisocyanate S?) (MDI) isomers, wherein the ratio of isomers is from about 65:35 to about 35:65; and at least one a diol compound having the following groups: (1) a hydroxyl group reactive with a mixture of MDI isomers of a polyisocyanate and (ii) at least one carboxylic acid group capable of forming a salt upon neutralization, wherein the at least one carboxylic acid group cannot Reacting with a mixture of MDI isomers of polyisocyanate. The precursor is then neutralized by, for example, triethylamine to form a salt and finally chain extended using a diamine chain extender and water to form Aqueous dispersions, which may include, for example, surfactants, antifoaming agents/antifoaming agents, antioxidants, Additives such as thickeners and combinations thereof. The MDI isomer mixture used in the anionic dispersion can achieve a reduction in the viscosity of the prepolymer without adding a solvent. The MDI isomer mixture is also used to reduce the reaction rate. Prepared by a batch process or a continuous process. When the diol is included in some embodiments, an alcohol including a hydroxyl group and a carboxylic acid group 123499.doc 16 200907139 can be described as an acid diol. Examples of available acid diols include 2 , 2 - di-m-acetic acid, 2,2-dimethylolpropionic acid (]:) 1 ^ 1 > VIII), 2,2-dihydroxymethylbutyric acid, 2,2-monomethylvalerate And their combinations. The nonionic film-forming dispersion of some embodiments comprises a prepolymer which is an isocyanate-terminated polyurethane prepolymer. Examples of suitable prepolymers are hydroxy-J-based polymers (for example polyols such as poly(tetramethylene-co-extension ethyl ether)-alcohol or poly(tetramethylene ether) diol and ethoxylate The reaction product of a mixture of polypropylene glycol and a diisocyanate such as 4,4,-methylenebis(phenylisocyanate). The prepolymer chain is then extended with water and dispersed in water or dispersed in water to extend the chain with water. The nonionic non-film forming dispersion of some embodiments comprises a prepolymer of a monoisocyanate-terminated polyurethane urethane prepolymer. The prepolymer is also a reaction of a polyol such as polybutadiene diol or poly(tetramethylene ether) diol with a diisocyanate such as 4, methylene bis(phenylisocyanate). product. The prepolymer can be chain extended using water in combination with a diamine bond extender such as ethylenediamine or an amine-functional crosslinker such as polyethylene. A hydrophilic or hydrophobic diol can be selected to produce a polymer powder having different water/oil absorption capabilities. Further, the powder particle control can be carried out by adjusting the prepolymer viscosity η Ί 7'4 ^ ν ??? π 哔 哔 预 预 预 预 预 预 预 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 To prepare such dispersions, the water-cooled portion can be more completely dispersed before the chain extension reaction begins. For example... can: to about "" low, including about 7 ° C or lower. "Some examples of a variety of sources are used in the case of liquids, such as steaming water, deionized l23499.d〇c • 17- 200907139 water or ultrapure water. For non-film forming or film forming dispersions, dispersions The average particle size of the medium particles is variable. As described above, one of the factors affecting the particle size is the viscosity of the prepolymer. The other factor is the dispersion speed, which can be, for example, about 5, 〇〇〇 rpm. Up to about 〇, 〇〇〇 rpm 'includes 7, 〇 0 rpm. The particle size range of the dispersions and powders of some embodiments includes about 400 micrometers (μm) or less, such as from about 0.01 μm to about 0.5 μm, 0.1 μηι to about 1.0 μηι, about 01 μηι to about 5 μηηη, about 〇15 μιη to about 0.65 μιη, and larger particles (for example, from about 1 〇μιη to about 1500 μm). In some embodiments a polyamino phthalate urea powder by dispersing the isocyanate-terminated prepolymer with high shear force in an aqueous medium containing a dispersing agent, a chain extender or a crosslinking agent, with or without a solvent. Preparation. High shear force is defined as a force sufficient to cause particles to be no greater than 5 microns. The prepolymer may be composed of a polyol or a polyol copolymer or a polyol mixture (for example, a polyether diol, a polyester diol, a polycarbonate diol, a polybutadiene diol or a hydrogenated derivative thereof, and a hydrazine). The base end group polydimethyl fluorene is reacted with an isocyanate (such as methylene bis(4-phenylisocyanate) (MDI)) to form an nc〇_end group prepolymer or ''capped Glycol " to prepare. In the polymer composition, the molar ratio of NCO / 〇H is between 1.2 and 5. An example of a chain extending agent is an aliphatic diamine such as ethylenediamine (EDA). When cross-linking of the powder is desired, the chain cross-linking agent can be an organic compound or polymer having at least three "- or amine-functional amine groups" capable of reacting with the foot groups. Dissolved or not: the right 撼C of the glutinous rice in the water, y, the organic / mixture of y (such as 1_methyl 2- oxapyridone 123499.doc -18- 200907139 (NMP) or xylene) can be used in Dilute the prepolymer before dispersion. The formed polyurethane urethane polymer fine particles dispersed in water can be used as such or separated into a solid powder by drying and drying. Alternatively, a spray process that also provides higher particle size control can be used. Some implementations may have a particle size that varies depending on their expectations. For example, the average particle size may be less than 1 mm (峨), and # includes an average particle diameter of less than (10) microns (μιη). In some embodiments, the polyurethane used in the preparation of the elastomeric powder comprises: a) a polyol or polyol copolymer or a polyol ketone having a number average molecular weight of from 500 to 5 Å, It includes, but is not limited to, polyttanol, polyglycol diol, poly lysine diol, polybutadiene diol or its chlorinated derivative, and base-based polydimethyl oxalate; b) Anisotropic acid vinegar, pots of t aliphatic diisocyanate, aromatic diisocyanate, cycloaliphatic diisocyanate, and c) aliphatic diamine (gp, _ (an amine chain) An extender) or a mixture or at least one amine-terminated polymer selected from the group consisting of aliphatic diamines and cycloaliphatic diamines G, each having from 2 to 13 carbon atoms. Or an organic compound or polymer having an organic hydrazine b to a primary or secondary amine group; and optionally, as a chain terminator. Examples of polyols that can be used in a certain class of A, 丨-&... include those having two or more of them, which are known from epoxy epoxide, tetrasulphate岵咗π oxime, oxyfuban, and 3_yinyl tetrahydroanthracene are obtained by ring-opening polymerization and/or copolymerization, or from multiple (four) (10), for example, every 12 carbon precursors have an iq /butanol or diol mixture, such as ethylene glycol, propylene, butylene glycol, hydrazine, 5-decanediol, hexanediol, neodecanediol, 123499.doc -19· 200907139 3-methyl-1, Polycondensation of 5-pentanediol, 1,7-heptanediol '1,8-octanediol, 1; 9-nonanediol, 1,10-nonanol and 1,12-edecyl alcohol obtain. By way of example, it may include a straight chain, difunctional polyether polyol, especially a poly(tetradecyl sulfonium 1) diol having a molecular weight of from about 1700 to 2100, such as a functionality of 2
Terathane® 1800(得自 Invista Si r.l· 〇f Wichita, KS andTerathane® 1800 (available from Invista Si r.l· 〇f Wichita, KS and
Wilmington,DE)。其他可用之市售聚醚多元酵之實例係在 市場上以 Acclaim® 4220N 自 Bayer,Pittsburgh,PA 及以 PLURACOL® 1062P 自 BASF,Wyandotte,MI 之購得者。其 他有用多元醇尤其包括四氫呋喃與環氧乙烷之共聚物、及 玉衣氧乙烧與私乳丙烧之共聚物。可組合一種以上類型之多 元醇以提供某些實施例之聚胺基甲酸酯脲組合物。舉例而 吕’當使用兩種不同多元醇時,其應以約25:75至約 75:25(包括約40:60至50:50)之比例組合。 可使用之聚醚多元醇之實例包括彼等具有兩個或兩個以 上羥基之醚二醇,其可藉由脂肪族多羧酸與每一分子中具 有不多於12個碳原子之低分子量多元醇、或其混合物之縮 聚來製備。適合多羧酸之實例係丙二酸、琥珀酸、戊二 酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸' 十一烷 一甲酸及十二烷二甲酸。適合用於製備聚醚多元醇之多元 醇只例係乙二醇、1,3_丙二醇、丁二醇、;[,5_戊二醇、 1,6-己二醇、新戊二醇、3_甲基戊二醇、L7 —庚二醇、 1,8-辛二醇、it壬二醇、ι,1〇_庚二醇及i,l2十二烷二 酉子。舉例而言,可包括一熔融溫度為約5〇c至約5(rc之直 鏈、雙官能團聚醚多元醇。 123499.doc -20- 200907139 可使用之聚碳酸酯多元醇之實例包括彼等具有兩個或兩 個以上經基之碳酸酯二醇’其藉由光氣、氣曱酸酯、碳酸 二烷酯或碳酸二丙烯酯與每一分子中具有不多於12個碳原 子之低分子量脂肪族多元醇、或其混合物之縮聚來製備。 適合用於製備聚碳酸酯多元醇之多元醇實例係二乙二醇、 1,3-丙二醇、M_ 丁二醇、i,5_戊二醇、150_己二醇、新戊 二醇、3-曱基-1,5_戊二醇、I?·庚二醇、•辛二醇、i,9_Wilmington, DE). Other examples of commercially available polyether polyols available on the market are Acclaim® 4220N from Bayer, Pittsburgh, PA and PLURACOL® 1062P from BASF, Wyandotte, MI. Other useful polyols include, inter alia, copolymers of tetrahydrofuran and ethylene oxide, and copolymers of acetylene and private emulsions. More than one type of polyol can be combined to provide the polyurethane urethane compositions of certain embodiments. For example, when two different polyols are used, they should be combined in a ratio of from about 25:75 to about 75:25 (including about 40:60 to 50:50). Examples of polyether polyols which may be used include those ether diols having two or more hydroxyl groups which may be formed by aliphatic polycarboxylic acids and low molecular weight having not more than 12 carbon atoms per molecule. It is prepared by polycondensation of a polyol, or a mixture thereof. Examples of suitable polycarboxylic acids are malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid 'undecane monocarboxylic acid and dodecanedicarboxylic acid. Polyols suitable for the preparation of polyether polyols are exemplified by ethylene glycol, 1,3-propanediol, butanediol, [,5-pentanediol, 1,6-hexanediol, neopentyl glycol, 3_methylpentanediol, L7-heptanediol, 1,8-octanediol, itodiol, iota, 1 庚 heptanediol, and i, l2 dodecane disaccharide. For example, a linear, difunctional polyether polyol having a melting temperature of from about 5 〇c to about 5 (rc) can be included. Examples of polycarbonate polyols that can be used include 123499.doc -20- 200907139 a carbonate diol having two or more trans-bases which is lower by phosgene, gas phthalate, dialkyl carbonate or dipropylene carbonate with no more than 12 carbon atoms per molecule A polycondensation of a molecular weight aliphatic polyol, or a mixture thereof, is prepared. Examples of polyols suitable for use in the preparation of polycarbonate polyols are diethylene glycol, 1,3-propanediol, M-butanediol, i,5-pentane Alcohol, 150_hexanediol, neopentyl glycol, 3-mercapto-1,5-pentanediol, I?·heptanediol, •octanediol, i,9_
壬二醇、U0-庚二醇及U2·十二烷二醇。舉例而言,可 包括一熔融溫度為約5t;至約5(TC之直鏈 '雙官能團聚碳 酸S旨多元醇。 適〇二異氰酸酯組份之實例係1,6~己二異氰酸酯、丨,12_ 十二烷二異氰酸酯、異氟爾酮二異氰酸酯、三甲基-六亞 甲基二異氰酸酯、2-甲基戊烷〗,^二異氰酸酯、環己烷二 異氰酸酯、亞甲基·雙(4_環已基異氰酸酯)、四甲基-二甲 苯二異氰酸酯、雙(異氰酸根曱基)環已烷、甲苯二異氰酸 酯、亞甲基雙(4·苯基異氰酸醋)、伸苯基二異氰酸醋、二 甲苯二異氰酸酯、及此等二異氰酸酯之混合物。舉例而 言,該二異氰酸酷可係芳香族二異氰酸酉旨,例如伸苯基二 異氰酸醋、甲苯二異氰酸γΤητ、 氰文酉日(TDI)、伸二甲苯基二異氰酸 酯、聯苯基二異氰酸酯、伸萘基二異氰酸酯、二苯基甲烷 二異氰酸S旨(MDI)(包括4,4,_亞甲基雙(苯基異氰酸醋)、 2,4'_亞甲基雙(苯基異氰醆酿)、及其組合)、及-或多種二 異氰酸酯之組合。 適合二胺組份(二胺鏈延長 劑)之實例係乙二胺 1,2-丙Decylene glycol, U0-heptanediol and U2·dodecanediol. For example, a melting temperature of about 5 t; to about 5 (TC's linear 'bifunctional polycarbonate S' polyol may be included. An example of a suitable diisocyanate component is 1,6-hexamethylene diisocyanate, hydrazine, 12_Dodecane diisocyanate, isophorone diisocyanate, trimethyl-hexamethylene diisocyanate, 2-methylpentane, diisocyanate, cyclohexane diisocyanate, methylene double (4 _cyclohexyl isocyanate), tetramethyl-xylene diisocyanate, bis(isocyanatoinyl)cyclohexane, toluene diisocyanate, methylene bis(4-phenylisocyanate), phenylene a mixture of diisocyanate, xylene diisocyanate, and such diisocyanates. For example, the diisocyanate may be an aromatic diisocyanate, such as phenyl diisocyanate, Toluene diisocyanate γΤητ, cyanide day (TDI), xylylene diisocyanate, biphenyl diisocyanate, stilbene diisocyanate, diphenylmethane diisocyanate S (MDI) (including 4, 4,_methylenebis(phenylisocyanate), 2,4'-methylenebis(phenyliso)醆 wine), and combinations thereof), and - a combination of two or more different cyanate esters suitable diamine component (diamine chain extender) of 1,2-propylene diamine-based examples
•2K 123499.doc 200907139 1,4-丁 二胺、 胺、1,3-丙二胺、2,2_二曱基-153_丙二胺、 1,5-戊二胺、六亞甲基二胺、1,7_庚二胺、-辛二胺、 1,9-壬二胺、u〇j二胺、十二烷二胺、曱基],5· 戊二胺、環己烷二胺、環己烷雙(甲胺)、異佛爾酮二胺、 伸二甲苯基二胺類、及亞甲基雙(環己二胺)。亦可使用兩 種或以上:胺之混合物。如上文所述,亦可包括水作為鍵 延長劑。• 2K 123499.doc 200907139 1,4-butanediamine, amine, 1,3-propanediamine, 2,2-didecyl-153-propylenediamine, 1,5-pentanediamine, hexamethylene Diamine, 1,7-heptanediamine, -octanediamine, 1,9-nonanediamine, u〇j diamine, dodecanediamine, mercapto], 5·pentanediamine, cyclohexane Amine, cyclohexane bis(methylamine), isophoronediamine, xylylene diamine, and methylene bis(cyclohexanediamine). It is also possible to use two or more: a mixture of amines. As mentioned above, water can also be included as a bond extender.
適合之胺端基聚合物之實例係雙(3_胺基丙基)端基之聚 二甲基矽氧烷、胺端基之聚(丙烯腈_共_ 丁二烯广雙㈠-胺 基丙基)端基之聚(乙二醇)、雙(2_胺基丙基)端基之聚(丙二 醇)、及雙(3-胺基丙基)端基之聚四氫咬喃。 具至少三個一級或二級胺基團之適合有機化合物或聚合 物之實例係叁-2-胺基乙基胺、聚(醯胺基胺)樹狀聚合物、 聚伸乙基亞胺、聚(乙烯基胺)、及聚(丙烯基胺)。 適合之單胺組份之實例包括一級烷基胺(諸如乙胺'丁 胺、己胺、環己胺、乙醇胺及2-胺基_2_甲基_丨_丙醇)、及 二級二烷基胺(諸如N,N-二乙胺、N_乙基·Ν·丙胺、队沁二 異丙胺、Ν-第三-丁基-Ν-甲胺、Ν_第三_丁基_Ν_节胺、 Ν,Ν-二環己基胺、Ν-乙基_Ν_異丙胺、沭第三_丁基異 丙胺、Ν-異丙基-Ν-環己基胺、Ν•乙基_Ν_環已基胺、Ν,Ν_ 二乙醇胺、及2,2,6,6-四甲基六氫吡啶)。 製造某些實施例之聚胺基甲酸酯脲粉末時,二醇首先與 二異氰酸酯在視情況存在一觸媒之情況下反應以形成 NCO-端基預聚物或"封端二醇”。此反應通常係在熔融形式 I23499.doc -22- 200907139 之均匀摻合混合物中於45至98t之溫度下加熱i小時至6小 時來貫施。各反應組份之量 '二醇之重量(Wgl)及二異氰 酸酯之重量(Wdi)係藉由封端比率(CR)來調節,此封端比 率疋義為一異氰酸酯與二醇之莫耳比率,如下所示: CR=(Wdi/MWdi)/(Wgl/MWgl) 其中Wdi係二異氰酸酯之分子量且河冒“係二醇之數量平 均为子S。根據本發明’封端比率介於1 2至5 〇之間,尤 其在1.5與3.0間。 當所有來自二醇分子之羥基(_〇H)皆被來自二異氰酸酯 之異氰酸酯(-NCO)基團消耗以形成胺基甲酸酯鍵結時封端 反應完成,此後形成一具末端NC〇基團之黏性聚胺基曱酸 酯預聚物。然後將此預聚物添加並分散至含有表面活性試 劑(例如分散劑及防泡劑/消泡劑)及視情況鏈延長劑(諸如 二胺)之水溶液中。或者,可在此預聚物分散至水介質中 之前用一諸如水溶性N-甲基吡咯啶酮(NMP)或水不溶性二 甲苯等有機溶劑稀釋。固體聚合物粒子係在高剪切力下在 分散期間並用水及/或二胺將鏈延長時形成。然後可將此 等聚胺基曱酸酯脲粒子過濾並乾燥。 由上述方法製備之聚胺基曱酸酯脲組合物令人驚訝地具 有良好水及油吸收性,尤其當應用於織物時。此對於抗污 特性尤為重要。在織物與某些實施例之聚胺基甲酸酯脲組 合物接觸後,聚胺基甲酸酯脲將自染點造成源吸收濕氣及 油且由此限制織物本身對其之吸收。 由於聚胺基曱酸酯脲組合物之吸收特性,其亦有助於延 123499.doc -23- 200907139 =與該組合物接觸之織物中的香氣實體化。 酸酿脲組合物對香油之吸收及隨後逐漸釋放之結:基甲 某—實施例之織物護理組合物可包括聚胺基 合物可添加於复中之舛舲畆 --a腦、,且 酸㈣組合物亦可呈^ 口物亦了呈诸如分散液或粉末等任一 者’此聚胺基甲酸酉旨服么人* 〆 制^田接添加至織物、至洗務 機H條用水(對於手洗而言)、或至自動乾燥以。 另外’該粉末或分散液可用作織物軟化劑之代替物以經 由家庭洗務賦予衣物抗污特性。織物軟化劑經常用於賦予 味或香乳且其次用於賦予織物柔軟性。當使用轉鼓 乾餘時織物軟化態樣並非必需的此乃因經轉鼓乾燥之織物 已非常柔軟。 某些實施例之洗滌劑組合物一般包含陰離子、非離子、 S夂鹼性兼備或兩性表面活性劑或其混合物且經常額外包含 一有機或無機增潔劑。 織物軟化劑一般包括一諸如四級銨鹽等活性組份。非環 狀四級銨鹽之實例包括牛脂基三甲基氯化銨;二牛脂基二 甲基氣化銨;二牛脂基二甲基銨甲基硫酸酯;二十六烷基 二甲基氯化銨,·二(氫化牛脂基)二甲基氣化銨;二十八烷 基二〒基氣化銨,·二二十烷基二甲基氯化銨;二二十二烷 基二甲基氣化銨;二(氫化牛脂基)二尹基銨甲基硫酸酯; 一十/、烷基二乙基氯化敍,·二十六烷基二甲基乙酸銨;二 牛脂基二丙基磷酸銨;二牛脂基二甲基硝酸銨及二(椰油_ 烷•基)二T基氯化敍。 123499.doc _24· 200907139 自然界中習用的某些實施例之織物護理組合物的其他可 選組伤一般以組合物或分散液重量計為約〇 . 〇 1 %至約 10%(包括自約〇.〇5至約5%,且包括自約2%至約4%)存在。 此等可選組份包括(但不限於)著色劑、香料、細菌抑制 劑、光凴劑、遮光劑、黏度調節劑、諸如黏土等固體形式 之織物處理劑、織物吸收增強劑、乳化劑、穩定劑、收縮 控制劑、去斑劑、殺菌劑、殺真菌劑、抗腐蝕劑等。其他 添加劑之實例包括防腐劑(例如乳酸)、抗氧化劑、顏料、 著色劑、香油、抗微生物劑(如銀)、活性成份(潤濕劑、 UV-掩蔽物)、表面活性劑、防泡劑/消泡劑、溶劑及諸如 此類’該f可在予員聚物分散前、鮮,或後#人聚胺基甲酸 酯脲組合物中。任何活性物質可單獨使用或與其他類似或 相異類型之添加劑組合使用。舉例而t,適合表面活性劑 包括彼等構自stepan公司’ Northfield,IL商標為 SOFT®及Stepante,者及購自KA〇有限公司商標為丁价_ 者。此等表面活性劑之組合可以任何適宜量使用,例如 50/5 0摻合物。 本發明之織物護理組合物可藉由習用方法製備。不需均 質化。一方便且令人滿意之方法係在約i 5〇卞下於水中製 備-軟化劑之預混合物’然後將其添加至其他組份之熱水 溶液中。溫度敏感性組份可在織物處理組合物冷卻至約^ 溫後添加。 某些實施例之織物護理組合物可藉由添加至習用家庭洗 衣作業之沖洗循環來使用。或者,該等織物護理組合物可 123499.doc -25- 200907139 直接添加至織物、 之部分或直接添加 或手洗 至洗滌 在洗滌循環之前添加至洗滌劑、 時作為洗滌劑或織物軟化组合物 用水中。 故寻織物護理組合物 J〜項议術T每知之形式施 用,例如粉末、液體、固體錠劑、囊封液體(舉例而士, 聚乙烯醇囊封之組合物)’或在使用自動乾燥器情況下以 不織物片施用。 某些實施例之織物護理組合物可以任何達成織物期望特 性所需之量添加。舉例而言’該等織物護理組合物以水性 沖洗浴或洗條用水的重量計可以約G G5%至約! 5%(舉例而 言,約0.2%至約1%)之量添加。 當以水性分散液存在時,某些實施例之聚胺基甲酸醋脲 組合物可以織物護理組合物重量計以約〇1 %至约鳩(舉例 而5約5%至約〗5%)存在於織物護理組合物中。當以粉末 存在時,該等聚胺基甲酸酯脲組合物可以織物護理組合物 重量s十以約0.1%至約2〇%(舉例而言約〇 5%至約1〇%,或約 1%至約5%)存在於織物護理組合物中。 或者,聚胺基甲酸酯脲粉末或分散液可作為織物護理組 合物之替代物而非織物護理組合物之組份添加,其中該聚 胺基甲酸S旨脲組合物可以ι〇0%添加。在此種情況下,該 聚胺基甲酸酯脲組合物可以沖洗用水或洗滌用水重量計以 約0.05%至約1.5〇/0(具體而言,自約〇 2%至約1%)之量直接 添加至洗滌用水或沖洗用水中。 藉由下述實例可更全面地展示本發明之特徵及優點,其 123499.doc -26· 200907139 而不應理解為 目的旨在闡釋本發明 明。 以任何方式限制本發 畔(由Invista,Γ丄提供)及 1圖价125臟形成且具有1之封端比率的封端二醇 預聚物係自試驗性LYCRA®氨綸生產線獲得。lycr^係Examples of suitable amine-terminated polymers are poly(3-aminopropyl) end group polydimethyl methoxy alkane, amine end group poly(acrylonitrile-co-butadiene broad bis(mono)-amine group Poly (ethylene glycol) end group poly(ethylene glycol), bis(2-aminopropyl) end group poly(propylene glycol), and bis(3-aminopropyl) end group polytetrahydroethylene. Examples of suitable organic compounds or polymers having at least three primary or secondary amine groups are anthracene-2-aminoethylamine, poly(decylamine) dendrimer, polyethyleneimine, Poly(vinylamine), and poly(propyleneamine). Examples of suitable monoamine components include primary alkylamines (such as ethylamine 'butylamine, hexylamine, cyclohexylamine, ethanolamine, and 2-amino-2-methyl-oxime-propanol), and secondary two Alkylamines (such as N,N-diethylamine, N-ethyl·anthraceneamine, quinone diisopropylamine, hydrazine-tertiary-butyl-hydrazine-methylamine, hydrazine_third-butyl-hydrazine) _ 节 、, Ν, Ν-dicyclohexylamine, Ν-ethyl Ν 异丙 isopropylamine, hydrazine tert-butyl isopropylamine, hydrazine-isopropyl-hydrazine-cyclohexylamine, hydrazine ethyl Ν _cyclohexylamine, hydrazine, hydrazine-diethanolamine, and 2,2,6,6-tetramethylhexahydropyridine). In the manufacture of the polyurethane urethane powder of certain embodiments, the diol is first reacted with a diisocyanate in the presence of a catalyst as appropriate to form an NCO-terminated prepolymer or "blocking diol" This reaction is usually carried out by heating in a homogeneous blending mixture of molten form I23499.doc -22-200907139 at a temperature of 45 to 98 t for 1 hour to 6 hours. The amount of each reaction component is the weight of the diol ( The weight of Wgl) and diisocyanate (Wdi) is adjusted by the capping ratio (CR), which is defined as the molar ratio of monoisocyanate to diol as follows: CR=(Wdi/MWdi) /(Wgl/MWgl) wherein Wdi is the molecular weight of the diisocyanate and the amount of the "diol" is the average S. According to the invention, the end capping ratio is between 12 and 5 Torr, especially between 1.5 and 3.0. The capping reaction is completed when all of the hydroxyl groups (_〇H) from the diol molecule are consumed by the isocyanate (-NCO) group from the diisocyanate to form a urethane bond, thereby forming a terminal NC thiol group. A viscous polyamino phthalate prepolymer. This prepolymer is then added and dispersed into an aqueous solution containing a surface active agent such as a dispersing agent and an antifoaming agent/antifoaming agent, and optionally a chain extender such as a diamine. Alternatively, it may be diluted with an organic solvent such as water-soluble N-methylpyrrolidone (NMP) or water-insoluble xylene before the prepolymer is dispersed in an aqueous medium. The solid polymer particles are formed under high shear under a period of dispersion and elongation of the chain with water and/or diamine. These polyaminophthalate urea particles can then be filtered and dried. The polyaminophthalate urea compositions prepared by the above process surprisingly have good water and oil absorbency, especially when applied to fabrics. This is especially important for stain resistance. After the fabric is contacted with the polyurethane urethane composition of certain embodiments, the polyurethane urethane causes the source to absorb moisture and oil from the dye point and thereby limit the absorption of the fabric itself. Due to the absorption characteristics of the polyamino phthalate urea composition, it also contributes to the extension of the aroma of the fabric in contact with the composition. 123499.doc -23- 200907139 = aroma of the fabric in contact with the composition. The absorption of the eucalyptus composition and the subsequent gradual release of the knot: the fabric care composition of the embodiment may comprise a polyamine compound which may be added to the sputum-a brain, and The acid (iv) composition may also be in the form of a dispersion or a powder, etc. 'This polyaminocarbazide is intended to serve the person* 〆 ^ ^ 接 添加 添加 添加 添加 添加 添加 添加 添加 添加 添加 添加 添加 添加 添加(for hand washing), or to automatic drying. Alternatively, the powder or dispersion can be used as a substitute for a fabric softener to impart stain resistance to the garment by household washing. Fabric softeners are often used to impart a taste or aroma and secondly to impart softness to the fabric. The softening of the fabric is not necessary when using the drum to dry. This is because the drum-dried fabric is very soft. The detergent compositions of certain embodiments typically comprise anionic, nonionic, S-alkaline or amphoteric surfactants or mixtures thereof and often additionally comprise an organic or inorganic builder. Fabric softeners typically include an active ingredient such as a quaternary ammonium salt. Examples of the acyclic quaternary ammonium salt include tallow trimethylammonium chloride; ditallow dimethyl ammonium sulfate; ditallow dimethyl ammonium methyl sulfate; hexadecyldimethyl chloride Ammonium, di(hydrogenated tallow) dimethyl vaporized ammonium; octadecyldiindenyl ammonium hydride, diicosyldimethylammonium chloride; didocosyldimethyl Base gasification ammonium; di(hydrogenated tallow) diinocyl ammonium methyl sulfate; tens/, alkyl diethyl chlorinated, · cetyl dimethyl ammonium acetate; ditallow dipropylene Ammonium phosphate; ditallow dimethyl ammonium nitrate and bis (coco® alkyl group) di-T-chloride. 123499.doc _24· 200907139 Other optional group wounds of fabric care compositions of certain embodiments that are conventional in nature are generally from about 〇1% to about 10% by weight of the composition or dispersion. .5 to about 5%, and including from about 2% to about 4%). Such optional components include, but are not limited to, colorants, perfumes, bacterial inhibitors, photoinhibitors, opacifiers, viscosity modifiers, fabric treatments in solid form such as clay, fabric absorption enhancers, emulsifiers, Stabilizers, shrinkage control agents, spot removers, fungicides, fungicides, anti-corrosion agents, and the like. Examples of other additives include preservatives (such as lactic acid), antioxidants, pigments, colorants, sesame oils, antimicrobial agents (such as silver), active ingredients (wetting agents, UV-masks), surfactants, antifoaming agents. / antifoaming agent, solvent and the like 'this f can be in the pre-dispersed, fresh, or post-human polyurethane urethane composition. Any active substance may be used alone or in combination with other similar or dissimilar types of additives. For example, t, suitable surfactants include those constructed by Stepan Inc.' Northfield, IL under the trademarks SOFT® and Stepante, and those purchased from KA〇 Co., Ltd. as Ding. Combinations of such surfactants can be used in any suitable amount, such as a 50/5 blend. The fabric care compositions of the present invention can be prepared by conventional methods. No need to homogenize. A convenient and satisfactory method is to prepare a pre-mix of the softener in water at about i 5 Torr and then add it to the hot water solution of the other components. The temperature sensitive component can be added after the fabric treatment composition has cooled to about . The fabric care compositions of certain embodiments can be used by a rinse cycle that is added to a conventional household laundry operation. Alternatively, the fabric care compositions can be added directly to the fabric, part or directly or hand-washed until the wash is added to the detergent prior to the wash cycle, as a detergent or fabric softening composition in water, 123499.doc -25-200907139 . Therefore, the fabric care composition J is to be applied in a form known per se, such as a powder, a liquid, a solid tablet, an encapsulated liquid (for example, a composition of polyvinyl alcohol encapsulated), or an automatic dryer is used. In the case of application without a fabric sheet. The fabric care compositions of certain embodiments can be added in any amount needed to achieve the desired properties of the fabric. For example, the fabric care compositions can be from about 5% to about 5% by weight of the aqueous rinse bath or wash water! 5% (for example, about 0.2% to about 1%) is added in an amount. The polyurethane urethane composition of certain embodiments may be present in an amount of from about 1% to about 鸠 (for example, from about 5 to about 5% by weight of the fabric care composition) when present in an aqueous dispersion. In fabric care compositions. When present in the form of a powder, the polyurethane urethane composition can be from about 0.1% to about 2% by weight of the fabric care composition (for example, from about 5% to about 1%, or about From 1% to about 5%) is present in the fabric care composition. Alternatively, the polyurethane urea powder or dispersion can be added as a substitute for the fabric care composition rather than as a component of the fabric care composition, wherein the polyuretic acid S urea composition can be added at 0% . In this case, the polyurethaneurea composition may be from about 0.05% to about 1.5 Å/0 (specifically, from about %2% to about 1%) by weight of the rinse water or wash water. The amount is added directly to the wash water or rinse water. The features and advantages of the present invention are more fully shown by the following examples, which are not intended to be construed as the description. The blocked diol prepolymer, which is formed in any way to limit the surface of the invention (provided by Invista, Γ丄) and 1 tidy 125 and has a capping ratio of 1 is obtained from a pilot LYCRA® spandex line. Lycr^
實例 實例1 由 Terathane mvista之氨綸的註冊商標。將3〇〇克此預聚物與15〇克NMp 溶劑於-塑料瓶内混合1G分鐘以降低黏度。將經稀釋之混 合物傾倒至一欲注入不銹鋼容器内之鋼管中以用於分散。 該容器含有2000克去離子水、3〇克丁 DET Nm表面活性劑 (購自Kansas City, Kansas之Harcros)及4·5克乙二胺鏈延長 劑,該等經預混合並冷卻至5。〇。在空氣壓力下將經稀釋 之預聚物以約40 psi藉助内徑為1/8英吋之管子注入以5〇〇〇 rpm運作之尚速實驗室分散器(型號hsm1〇〇lc,購自EXAMPLES Example 1 A registered trademark of Spandex by Terathane mvista. 3 g of this prepolymer was mixed with 15 g of NMp solvent in a -plastic bottle for 1 G minutes to reduce the viscosity. The diluted mixture is poured into a steel tube to be poured into a stainless steel container for dispersion. The vessel contained 2000 grams of deionized water, 3 gram of DET Nm surfactant (Harcors available from Kansas City, Kansas) and 4.5 grams of ethylenediamine chain extender, which were premixed and cooled to 5. Hey. The diluted prepolymer was injected at about 40 psi with a tube of 1/8 inch internal diameter under air pressure into a laboratory disperser operated at 5 rpm (model hsm1〇〇lc, purchased from
Hauppauge,New York之Charles Ross & Son公司)。在 15分 鐘之内完成經稀釋預聚物的添加,將所形成之乳白色分散 液再繼續分散5分鐘。容器之反向稱重得出添加至分散液 中之經稀釋封端二醇總量係328克,相當於將2 1 8.7克封端 二醇預聚物添加至分散液中。將3克Additive 65泡殊控制 劑(講自Midland,Michigan之Dow Corning)添加至該分散液 中’並將分散液以5000 rpm再混合30分鐘後傾倒至塑料瓶 中〇 借助Microtrac X100粒徑分析儀(Leeds,Northrup)經測定 123499.doc -27· 200907139 其中95%之粒子小於 分散液之平均粒徑為52.83微米 202.6微米。 實例2 使用與實m相同之成份及分散程序,只是經稀釋之預 聚物分散至水混合物後添加4·5克乙二胺鏈延長劑。容器 之反向稱重得出添加至分散液之經稀釋封端二醇總量係 ⑵克,相當於將219克封端二醇預聚物添加至分散液中。 分散液之平均粒徑經測定為33,45微米,其中之粒子小 於64.91彳政米。固體聚合物粒子分離時不形成薄膜。 實例3 ' 封端二醇預聚物係藉由500克Kras〇l® HLB 2000二醇(由 Extern,PAiSartomer有限公司提供 1 2 5MDR於90 C在2000毫升配備有加熱夾套及機械攪拌器 之反應爸内反應120分鐘來製備。此反應係於一充氮乾燥 箱内實施。反應後,預聚物具有2 98重量%之NC〇基團, 如藉由滴定法所測定。將此預聚物傾倒至一欲注入不銹鋼 容器内之鋼管中以用於分散。在室溫下將去離子水(2〇〇〇 克)與30克T DET N14表面活性劑(購自Kansas City,Kansas 之Harcros)及3克Additive 65泡沫控制劑(購自Midland, Michigan之Dow Corning)於容器内混合。在空氣壓力下將 該預聚物以約80 psi藉助内徑為1/8英吋之管子注入以5000 rpm運行之高速實驗室分散器(型號HSM-100LC,購自 Hauppauge,New York 之 Charles Ross & Son公司)。在15 分鐘之内完成經稀釋預聚物之添加,將所形成之乳白色分 123499.doc -28- 200907139 散液再繼續分散5分鐘。容器之反向稱重得出添加至分散 液中之經稀釋封端二醇總量係422克。將4·5克乙二胺鏈延 長劑添加至分散液中且將混合物以5〇〇〇 rpm再混合30分 鐘。所形成分散液之平均粒徑經測定為49.8 1微米,其中 95%之粒子小於3〇9.7微米。 實例4 該等程序與實例3相同,只是使用250克Terathane® 1800 二醇及25 0克Krasol® HLB 2000二醇之二醇混合物以形成預 聚物。將總共465克預聚物分散。所形成之分散液平均粒 徑經測定為13.67微米,其中95%之粒子小於38.26微米。 實例5 預聚物之製備係在具有氮氣氣氛之手套箱内進行。向 2000毫升配備有空氣壓力驅動攪拌器、加熱夾套、及熱電 偶溫度量測器之Pyrex®玻璃反應釜内填充約382.5克 Terathane® 1800二醇(購自 lnvista,r丄,Wichita,Ks)及 約12.5克2,2-二羥甲基丙酸(〇河卩八)。攪拌的同時將此混合 物加熱至約5(TC,然後添加約105克Lupranate® MI二異氰 酸酯(購自BASF,Wyandotte,Michigan)。然後持續攪掉的 同時將反應混合物加熱至約90。(:並且在約90。(:下保持約 120分鐘,此後反應完成,此時混合物之% NC〇降至一穩 定值,該值與具有異氰酸酯端基之預聚物的計算值一致(% NCO目標值為1.914)。預聚物之黏度係根據astm D1343- 69之一般方法使用於約40。(:下運行之DV-8型落球黏度計 (由Duratech公司,Waynesboro, VA_出售)來測定。封端二 123499.doc •29- 200907139 醇預聚物之總異氰酸酯部分含量(以NCO基團之重量百分 比計)係藉由 S. Siggia,"Quantitative Organic Analysis viaHauppauge, Charles Ross & Son Company, New York). The addition of the diluted prepolymer was completed within 15 minutes, and the resulting milky white dispersion was further dispersed for 5 minutes. The reverse weighing of the vessel gave a total of 328 grams of the diluted capped glycol added to the dispersion, corresponding to the addition of 2 1 8.7 grams of blocked diol prepolymer to the dispersion. Add 3 grams of Additive 65 bubble control agent (from Dow Corning, Midland, Michigan) to the dispersion and mix the dispersion at 5000 rpm for 30 minutes, then pour into a plastic bottle and analyze with Microtrac X100 particle size. The instrument (Leeds, Northrup) was determined to have a mean particle size of 52.83 microns and 202.6 microns. Example 2 The same ingredients and dispersion procedure as in the real m were used except that the diluted prepolymer was dispersed in the water mixture and 4.55 g of ethylenediamine chain extender was added. The reverse weighing of the vessel gave a total of (2) grams of the diluted capped glycol added to the dispersion, corresponding to the addition of 219 grams of capped glycol prepolymer to the dispersion. The average particle size of the dispersion was determined to be 33, 45 μm, and the particles were smaller than 64.91 彳. No solid film is formed when the solid polymer particles are separated. Example 3 'The capped glycol prepolymer was passed through 500 g of Kras〇l® HLB 2000 diol (provided by Extern, PAiSartomer Ltd. 1 25 MDR at 90 C in 2000 ml equipped with a heating jacket and mechanical stirrer) The reaction was carried out by reacting in the dad for 120 minutes. The reaction was carried out in a nitrogen-filled dry box. After the reaction, the prepolymer had a hydroxyl group of 298% by weight, as determined by titration. Pour into a steel tube to be poured into a stainless steel container for dispersion. Deionized water (2 gram) and 30 grams of T DET N14 surfactant at room temperature (Harscos from Kansas City, Kansas) And 3 grams of Additive 65 foam control agent (available from Dow Corning, Midland, Michigan) was mixed in a container. The prepolymer was injected at about 80 psi with a tube having an inner diameter of 1/8 inch under air pressure. High-speed laboratory disperser (model HSM-100LC, available from Charles Ross & Son Company, Hauppauge, New York) running at 5000 rpm. Adding the diluted prepolymer in 15 minutes, the resulting milky white 123499.doc -28- 200907139 Dispersion Disperse for 5 minutes. The reverse weighing of the container gives 422 grams of the total amount of diluted capped glycol added to the dispersion. 4. 5 grams of ethylenediamine chain extender is added to the dispersion and the mixture is The mixture was further mixed for 30 minutes at 5 rpm. The average particle diameter of the resulting dispersion was determined to be 49.8 1 μm, of which 95% of the particles were less than 3 〇 9.7 μm. Example 4 The procedure was the same as in Example 3 except that 250 g was used. A mixture of Terathane® 1800 diol and 250 grams of Krasol® HLB 2000 diol to form a prepolymer. A total of 465 grams of prepolymer was dispersed. The average particle size of the resulting dispersion was determined to be 13.67 microns, 95 of which % of the particles are less than 38.26 microns. Example 5 Prepolymer preparation was carried out in a glove box with a nitrogen atmosphere. Pyrex® equipped with an air pressure driven stirrer, heating jacket, and thermocouple temperature gauge to 2000 ml The glass reactor was filled with approximately 382.5 grams of Terathane® 1800 diol (available from lnvista, r丄, Wichita, Ks) and approximately 12.5 grams of 2,2-dimethylolpropionic acid (〇河卩八). This mixture is heated to about 5 (TC, then added 105 g Lupranate® MI diisocyanate (commercially available from BASF, Wyandotte, Michigan). Then while continuing stirring away reaction mixture was heated to about 90. (: and at about 90. (: for about 120 minutes, after which the reaction is completed, at which time the % of the mixture is reduced to a stable value, which is consistent with the calculated value of the prepolymer having isocyanate end groups (% NCO) The target value is 1.914. The viscosity of the prepolymer is about 40 for the general method of astm D1343-69. (: DV-8 type ball viscous meter (sold by Duratech, Waynesboro, VA_) Blocking two 123499.doc • 29- 200907139 The total isocyanate content of the alcohol prepolymer (in weight percent of NCO groups) is determined by S. Siggia, "Quantitative Organic Analysis via
Functional Group" ’ 第三版,Wiley & Sons,New York,第 559-561頁(1963)(其全文以引用方式併入本文中)中之方法 量測。 實例6 根據貫例5所述之程序及組合物製備之無溶劑預聚物用 於製造本發明之聚胺基甲酸酯脲水性分散液。 向2,000毫升不銹鋼燒杯中填充約700克去離子水、約15 克十二烧基苯續酸鈉(SDBS)、及約1〇克三乙胺(TEA)。然 後用冰/水將此混合物冷卻至約5。〇並用一具有轉子/定子混 合頭之尚剪切實驗室混合器(Ross,100LC型)以約5,〇〇〇 rpm混合約3〇秒鐘。將以實例i之方法所製備並包含於金屬 管狀圓同内之黏性預聚物藉助撓性管同時施加空氣壓力添 加至於水溶液中之混合頭底部。預聚物溫度保持在介於約 5〇°C與約70°C之間。將經擠出之預聚物流分散並在約5〇〇〇 rpm之持續混合下用水使其鏈延長。在約5〇分鐘内,將總 量為約540克之預聚物引入並分散至水中。預聚物添加並 分散後立即向分散混合物中填充約2克AddiUve 65(購自Functional Group" ' Third Edition, Wiley & Sons, New York, pp. 559-561 (1963), the entire disclosure of which is incorporated herein by reference. Example 6 A solventless prepolymer prepared according to the procedure and composition described in Example 5 was used to produce an aqueous polyurethaneurea dispersion of the present invention. A 2,000 ml stainless steel beaker was filled with about 700 grams of deionized water, about 15 grams of sodium dodecyl benzoate (SDBS), and about 1 gram of triethylamine (TEA). The mixture was then cooled to about 5 with ice/water. The mixture was mixed with a still shearing laboratory mixer (Ross, Model 100LC) having a rotor/stator mixing head at about 5, rpm for about 3 seconds. The viscous prepolymer prepared by the method of Example i and contained in the metal tubular circle was simultaneously applied to the bottom of the mixing head in the aqueous solution by means of a flexible tube while applying air pressure. The prepolymer temperature is maintained between about 5 ° C and about 70 ° C. The extruded prepolymer stream was dispersed and the chain was extended with water with continuous mixing at about 5 rpm. A prepolymer having a total amount of about 540 g was introduced and dispersed into water in about 5 minutes. Immediately after the prepolymer was added and dispersed, about 2 g of AddiUve 65 was filled into the dispersion mixture (purchased from
Dow Corning®,Midland Michigan)。然後將反應混合物再 混合約30分鐘,隨後添加約6克二乙胺(DEA)並額外混合。 所得無溶劑之水性分散液係乳白色且穩定。 實例7 125MDR(購自 Dow公 自 Terathane® 1800 二醇及 Is〇nate® 123499.doc -30- 200907139 司,Midland,Michigan)所形成且具有1 688封端比率之封 鈿一醇預聚物係得自商業LYCRA®氨綸生產線。LYCRA® 係Inv1Sta之氨綸的注冊商標。將3〇〇克此預聚物與15〇克 NMP备劑於一塑料瓶内混合丨〇分鐘以降低黏度。將經稀釋 混合物傾倒至一欲注入不銹鋼容器内之鋼管中以用於分 散。该容含有2000克去離子水、3〇克τ DET N14表面活 性劑(購自Kansas City,Kansas之Harcr〇s)及3克乙二胺鏈延 長劑,該等經預混合並冷卻至5 °c。在空氣壓力下將經稀 釋之預聚物以約40 psi藉助内徑為1/8英吋之管子注入以 5 000 rpm運作之高速實驗室分散器(型號hSm-1〇〇LC,購 自 Hauppange,New York之 Charles R0SS & Son公司)。在 15 分鐘之内完成經稀釋預聚物之添加,將所形成之乳白色分 散液再繼續分散5分鐘。容器之反向稱重得出添加至分散 液中之經稀釋封端二醇總量係347克,相當於將23 1克封端 二醇預聚物添加至分散液中。將3克Additive 65泡沫控制 劑(購自Midland,Michigan之Dow Corning)添加至分散液中 並將分散液以5000 rpm再混合3〇分鐘後傾倒至塑料瓶中。 借助1^(^〇的〇乂100粒徑分析儀(1^6(18,]^〇1^1>1;11))測定分 散液之平均粒徑為32.59微米,其中95%之粒子低於65.98 微米。使用一 Buchner漏斗與Whatman®遽紙在低壓下過淚 該等固體預聚物粒子’用水沖洗濾餅三次,並於60-651 下乾燥4小時。顆該等粒子在過濾或乾燥期間不形成薄 膜。借助實驗室Waring®混合器(由Dynamics公司,NewDow Corning®, Midland Michigan). The reaction mixture was then mixed for a further 30 minutes, followed by the addition of about 6 grams of diethylamine (DEA) and additional mixing. The resulting solvent-free aqueous dispersion is milky white and stable. Example 7 125MDR (available from Dow Corporation from Terathane® 1800 diol and Is〇nate® 123499.doc -30-200907139, Midland, Michigan) and a 1 688 capping ratio of the succinyl alcohol prepolymer system From the commercial LYCRA® spandex production line. LYCRA® is a registered trademark of Inv1Sta's spandex. Mix 3 g of this prepolymer with 15 g of NMP in a plastic bottle for a few minutes to reduce the viscosity. The diluted mixture is poured into a steel tube to be poured into a stainless steel container for dispersion. The volume contains 2000 grams of deionized water, 3 grams of τ DET N14 surfactant (purchased from Kansas City, Kansas, Harcr〇s) and 3 grams of ethylenediamine chain extender, which are premixed and cooled to 5 ° c. The diluted prepolymer was injected into a high speed laboratory disperser operating at 5 000 rpm with a diameter of 1/8 inch at about 40 psi under air pressure (model hSm-1〇〇LC, available from Hauppange , Charles R0SS & Son, New York.) The addition of the diluted prepolymer was completed in 15 minutes, and the resulting milky white dispersion was further dispersed for 5 minutes. The reverse weighing of the vessel gave a total of 347 grams of the diluted capped glycol added to the dispersion, corresponding to the addition of 23 1 grams of the capped glycol prepolymer to the dispersion. 3 grams of Additive 65 foam control agent (available from Dow Corning, Midland, Michigan) was added to the dispersion and the dispersion was mixed for another 3 minutes at 5000 rpm and poured into a plastic bottle. The average particle size of the dispersion was determined to be 32.59 μm by using a ^100 particle size analyzer (1^6(18,]^〇1^1>1;11)), wherein 95% of the particles were low. At 65.98 microns, the solid prepolymer particles were rinsed three times with a Buchner funnel and Whatman® crepe paper under low pressure and dried at 60-651 for 4 hours. The particles were filtered or dried. No film is formed during the period. With the laboratory Waring® mixer (by Dynamics, New
Hartford,Connecticut製造之Blender 700 33BL79型)容易地 123499.doc -31 · 200907139 將經乾燥之濾餅磨成微粉 可使用習用乾焊〜, 業實踐中,忒專固體粒子 如藉由霧乾燥)直接自分散液分離。 子量及85200 丄"^燥叙末具有352,550之重量平均分 子里及85,200之數量平均分子量。 刀 實例8 用中使用與實例7中相同之組份及分散程序,只是將 長”二醇預聚物之溶劑改為三甲苯并將乙 延長劑之量增$ 4 ς ^ 月女鏈 … 曰至4·5克。容器之反向稱重得出添加至分散 液之經稀釋封端二 刀散 醇預聚物^ 私、〜里係339克,相當於將226克封端二 予預欷物添加至分散液中。 氮测疋分散液之平均粒徑為22 88微米,其"外粒子小 參6.97微米。固體聚合物粒子分離時不形成薄膜。 實例9 貫=9中使用與實例7中相同之組份及分散程序,只是將 乙月女鏈延長劑替換為等量之具支鍵聚伸乙基亞胺(藉由 啦測定Μη約為_,得自杨地)。容器之反向稱重得出 外加至分散液中之經稀釋封端二醇總量係34〇克,相當於 將227克封端二醇預聚物添加至分散液中。 ’…則疋分散液之平均粒徑為58.12微米,其中95%粒子小 ;8.5微米。固體聚合物粒子分離時不形成薄膜。 實例10 使用—具乾燥氮氣氣氛之手套箱製備預聚物。向兩個單 獨:配備有空氣壓力驅動攪拌器、加熱夾套、及熱電偶溫 度里測器之2000毫升Pyrex®玻璃反應爸内各填充22〇 〇克 123499.doc •32- 200907139Hartford, Connecticut, manufactured by Blender 700 33BL79) easily 123499.doc -31 · 200907139 The dried filter cake can be ground into fine powder using conventional dry welding ~, in practice, 忒 special solid particles such as by fog drying) directly Separation from the dispersion. The sub-quantity and 85,200 丄"^ dry ends have a weight average molecular weight of 352,550 and an average molecular weight of 85,200. Knife Example 8 The same components and dispersion procedures as in Example 7 were used, except that the solvent of the long "diol prepolymer was changed to trimethylbenzene and the amount of the ethyl extender was increased by $4 ς ^ month female chain... 曰Up to 4.5 gram. The reverse weighing of the container results in the diluted end-capped second-knife alcohol prepolymer added to the dispersion, 339 grams, which is equivalent to 226 grams of the end of the two The material is added to the dispersion. The average particle size of the nitrogen-measuring dispersion is 22 88 μm, and the outer particle is 6.97 μm. The solid polymer particles are not formed into a film when separated. Example 9 Use and Example of 9 The same components and dispersing procedures in 7 except that the female model chain extender of the month is replaced by an equivalent amount of the branched polyethylenimine (determined by Μη, which is obtained from Yangdi). Reverse weighing gives the total amount of diluted capped glycol added to the dispersion 34 g, which corresponds to the addition of 227 g of capped glycol prepolymer to the dispersion. '...then the dispersion The average particle size is 58.12 microns, of which 95% of the particles are small; 8.5 microns. The solid polymer particles do not form a film when separated. 10 Prepare the prepolymer using a glove box with a dry nitrogen atmosphere. Fill the two separate: 2000 ml Pyrex® glass with an air pressure driven stirrer, heating jacket, and thermocouple temperature detector. 22 gram 123499.doc •32- 200907139
Terathane 1 800 -舻广诚 & τ , —醇(購自 Invista)及 220.0 克 Pluracol® HP 4000D二醇(講自 b a ςρ、 目BASF) °撹拌的同時將此二醇混合物加熱 至 50 C,Ik 後添加 75 〇3 克 125MDR(購自Terathane 1 800 - 舻广诚 & τ, - alcohol (available from Invista) and 220.0 grams of Pluracol® HP 4000D diol (from ba ςρ, 目BASF) ° while mixing the diol mixture to 50 C, Add 75 〇 3 g 125MDR after Ik (purchased from
Chemical)。然後持續攪拌的同時將該反應混合物加熱至卯 C並在9G C下維持12G分鐘。將樣品自反應器取出,且經 測定分別具有2.170及2.169% NCO,如藉由S. Siggia, Quantitative Organic Analysis via Functional Group”,第 二版,Wiley & Sons,New York,第 559-561 頁(1963)之方 法所量測。 向3 000毫升不銹鋼燒杯中填充16〇〇克去離子水、15克τ DET N14 表面活性劑(購自 Kansas Chy,Kansas之 Harcr〇s)及 5克Additive 65(購自Dow Corning)。然後用冰/水將此混合 物冷卻至10。(:並用一具有轉子/定子混合頭之高剪切實驗 室混合器(Ross,100LC型)以5000 rpm混合30秒鐘。將如上 於兩個反應器内製備之黏性預聚物倒至金屬管狀圓筒中並 藉助撓性管同時施加空氣壓力將其添加至於水溶液中之混 合頭底部。預聚物溫度保持在介於50-70。(:之間。將經擠 出之預聚物流分散並於5000 rpm之持續混合下用水進行鏈 延長。在5分鐘内’將總量為6 1 6克之預聚物引入並分散至 水中。預聚物添加並分散後,將分散混合物再混合4〇分 鐘。所得無溶劑之水性分散液係乳白至淡藍色,其具有 28.84重量%之固體含量及44厘泊之黏度。將分散液洗铸於 1乙稀薄片上並且於通風廚中在環境條件下乾燥過夜以形 成一彈性連續膜。藉由GPC量測,此薄臈具有127 9〇〇之重 123499.doc •33- 200907139 量平均分子量及41,000之數量平均分子量。 實例11 程序與條件基本與上述實例1 0相同,只是將表面活性劑 改為 Bio-soft® Nl-9(購自 Stepan of Northfield,Illinois)。將 來自兩個反應器具有2.1 56及2.136% NCO總共640克預聚物 分散至水中。所形成之不含溶劑分散液具有26.12%之固體 含量及5 1厘泊之黏度。該澆鑄且經乾燥彈性膜具有 133,900之重量平均分子量及44,400之數量平均分子量。 實例12 使用一具乾燥氮氣氣氛之手套箱製備預聚物。向兩個單 獨的配備有空氣壓力驅動攪拌器、加熱夾套、及熱電偶溫 度量測器之2000毫升pyrex®玻璃反應釜内各填充440.0克Chemical). The reaction mixture was then heated to 卯 C while continuing to stir and maintained at 9 G C for 12 G minutes. The samples were taken from the reactor and determined to have 2.170 and 2.169% NCO, respectively, as by S. Siggia, Quantitative Organic Analysis via Functional Group", Second Edition, Wiley & Sons, New York, pages 559-561. Measured by the method of (1963). Fill a 3 000 ml stainless steel beaker with 16 g of deionized water, 15 g of τ DET N14 surfactant (purchased from Kansas Chy, Kansas Harcr〇s) and 5 g of Additive 65 (purchased from Dow Corning). The mixture was then cooled to 10 with ice/water. (: and mixed with a high shear laboratory mixer (Ross, Model 100LC) with a rotor/stator mixing head at 5000 rpm for 30 seconds. The viscous prepolymer prepared in the two reactors as above was poured into a metal tubular cylinder and added to the bottom of the mixing head in the aqueous solution by means of a flexible tube while applying air pressure. The temperature of the prepolymer was kept at a temperature. 50-70. (Between: The extruded prepolymer stream was dispersed and chain extended with water at 5000 rpm with continuous mixing. In a total of 6 16 g of prepolymer introduced and dispersed in 5 minutes To the water. Prepolymer addition After dispersion, the dispersion mixture was further mixed for 4 minutes. The resulting solvent-free aqueous dispersion was milky white to pale blue with a solid content of 28.84% by weight and a viscosity of 44 centipoise. The dispersion was washed in 1 estro It was dried on-chip and in a ventilated kitchen under ambient conditions to form an elastic continuous film. The weight of the enamel was 127 9 123 by the GPC measurement. 123499.doc • 33- 200907139 The average molecular weight and 41,000 Number average molecular weight. Example 11 Procedures and conditions were essentially the same as in Example 10 above, except that the surfactant was changed to Bio-soft® Nl-9 (purchased from Stepan of Northfield, Illinois). There will be 2.1 56 from both reactors. And 2.136% NCO total 640 grams of prepolymer dispersed into water. The resulting solvent-free dispersion has a solids content of 26.12% and a viscosity of 51 centipoise. The cast and dried elastic film has a weight average molecular weight of 133,900 and Number average molecular weight of 44,400. Example 12 A prepolymer was prepared using a glove box with a dry nitrogen atmosphere. Two separate air-driven agitators, heating jackets, Each filled the 2,000 ml glass reactor pyrex® thermocouple temperature measuring device measures the 440.0 g
Terathane® 1800二醇(購自 invista)及 440.0 克 Plurac〇i® 1〇62 二醇(購自BASF)。攪拌的同時將此二醇混合物加熱至5〇 C ’隨後添加 150.0 克 Isonate® 125MDR(購自 Dow Chemical)。然後持續攪拌的同時將該反應混合物加熱至卯 °C並在90°C下維持120分鐘。將樣品自反應器取出,且經 測定分別具有約2% NCO,如藉由s· Siggia,”QuantitativeTerathane® 1800 diol (available from invista) and 440.0 grams of Plurac〇i® 1〇62 diol (available from BASF). This diol mixture was heated to 5 〇 C ' while stirring, followed by the addition of 150.0 g of Isonate® 125 MDR (available from Dow Chemical). The reaction mixture was then heated to 卯 ° C while continuing to stir and maintained at 90 ° C for 120 minutes. The sample was taken out of the reactor and determined to have about 2% NCO, respectively, as by s· Siggia,” Quantitative
Organic Analysis Via Functi〇nal Gr〇up”,第三版,Wiley &Organic Analysis Via Functi〇nal Gr〇up", Third Edition, Wiley &
Sons’NewYork,第 559_561頁(1963)之方法所量測。 向3000*升不銹鋼燒杯中填充15〇〇克冷卻至約之超 純水、25.9 克 Bi0-S0ft® Ν25·9 及 25 9 克 stepantex<& ντ_9〇(二 者均講自Stepan公司)及1〇克Additive 65(賜自D〇w 然後用-具有轉子以子混合頭之高剪切實驗室 123499.doc 34、 200907139 混合器(Ross ’ l〇〇LC型)將此混合物以7000 rpm混合30秒 鐘。將如上於兩個反應器内製備之黏性預聚物倒至金屬管 狀圓筒中並藉助撓性管同時施加空氣壓力將其添加至於水 溶液中之混合頭底部。預聚物溫度保持在介於5〇_7〇之 間。將經擠出之預聚物流分散並於7〇〇〇 rpm之持續混合下 用水再進行鏈延長2分鐘。此後添加2.33克PURAC®乳酸防 腐劑。所得不含溶劑之水性分散液係乳白至淡藍色,其具 有35重量%之固體含量。 實例13 使用具乾综氮氣氣氛之手套箱製備預聚物。向兩個單 獨的配備有空氣壓力驅動攪拌器、加熱夾套、及熱電偶溫 度量測器之2000毫升Pyrex®玻璃反應釜内各填充440.0克 Terathane® 1800 二醇(購自 invista)及 44〇(^plurac〇1® 1〇62 二醇(購自BASF)。攪拌的同時將此二醇混合物加熱至5〇 °C ’ 隨後添加 150.0 克 lsonate® 125MDR(購自 Dow Chemical)。然後持續攪拌的同時將該反應混合物加熱至9〇 °C並維持在90°C下達120分鐘。將樣品自反應器取出,且 經測定分別含有2% NCO,此係藉由S. Siggia,Sons’ New York, pp. 559_561 (1963) measures. Fill a 3000*l stainless steel beaker with 15 grams of water to about ultrapure water, 25.9 grams of Bi0-S0ft® Ν25·9 and 25 9 grams of stepantex<& ντ_9〇 (both from Stepan) and 1 Add克 Additive 65 (given from D〇w and then used - high shear laboratory with rotor with sub-mixing head 123499.doc 34, 200907139 mixer (Ross 'l〇〇LC type) mix this mixture at 7000 rpm 30 The viscous prepolymer prepared in the two reactors as above was poured into a metal tubular cylinder and added to the bottom of the mixing head in the aqueous solution by means of a flexible tube while applying air pressure. The temperature of the prepolymer was kept at Between 5〇_7〇. The extruded prepolymer stream was dispersed and subjected to chain extension for 2 minutes with continuous mixing at 7 rpm, after which 2.33 g of PURAC® lactic acid preservative was added. The solvent-containing aqueous dispersion was milky white to light blue with a solids content of 35% by weight.Example 13 A prepolymer was prepared using a glove box with a dry nitrogen atmosphere. Two separate air pressure driven agitators were provided. , heating jacket, and thermoelectric The temperature measuring device's 2000 ml Pyrex® glass reactor was filled with 440.0 g of Terathane® 1800 diol (purchased from invista) and 44 〇 (^plurac〇1® 1〇62 diol (purchased from BASF). The diol mixture was heated to 5 ° C. Then 150.0 grams of lsonate® 125MDR (available from Dow Chemical) was added. The reaction mixture was then heated to 9 ° C while maintaining stirring at 90 ° C for 120 minutes. The sample was taken out of the reactor and determined to contain 2% NCO, respectively, by S. Siggia,
Quantitative Organic Analysis via Functional Group",第 二版,Wiley & Sons,New York,第 559-561 頁(1963)之方 法所量測。 向3000毫升不銹鋼燒杯中填充15〇〇克冷卻至約1(Γ(:之超 純水、25.9克則0-8〇反《>125_9(購自以邛抓公司)及25 9克Quantitative Organic Analysis via Functional Group", Second Edition, Wiley & Sons, New York, pp. 559-561 (1963). Fill 15 ml of stainless steel beaker into a 3000 ml to cool to about 1 (Γ (: ultra pure water, 25.9 g is 0-8 〇 anti-> 125_9 (purchased from 邛 scratch company) and 25 9 g
Tetranyl® L1/90L(購自 Kao Corporation)及 10克 Additive 123499.doc -35- 200907139 65(購自Dow C〇rning)。然後用—具有轉子/定子混合頭之 高剪切實驗室混合器(R〇ss,刚LC型)將此混合物以7嶋 rpm混合30秒鐘。將如上於兩個反應器内製備之黏性預聚 物倒至金屬管狀圓Μ中並藉助撓性管同時施加空氣壓力將 其添加至於水溶液中之混合頭底部。預聚物溫度保持在介 於50-70°C之間。將經擠出之預聚物流分散並於7〇〇〇 之持續混合下用水再進行鏈延長2分鐘。此後添加2 33克 PURAC乳酸防腐劑。所得不含溶劑之水性分散液係乳白 至淡藍色’其具有35重量%之固體含量。 實例14 使用一具乾燥氮氣氣氛之手套箱製備預聚物。向兩個單 獨的配備有空氣壓力驅動攪拌器、加熱夾套及熱電偶溫度 量測器之2000毫升Pyrex®玻璃反應釜内各填充44〇 〇克Tetranyl® L1/90L (available from Kao Corporation) and 10 grams of Additive 123499.doc -35- 200907139 65 (available from Dow C〇rning). This mixture was then mixed at 7 rpm for 30 seconds using a high shear laboratory mixer (R〇ss, just LC type) with a rotor/stator mixing head. The viscous prepolymer prepared in the above two reactors was poured into a metal tubular round crucible and added to the bottom of the mixing head in the aqueous solution by means of a flexible tube while applying air pressure. The prepolymer temperature is maintained between 50 and 70 °C. The extruded prepolymer stream was dispersed and subjected to chain extension for 2 minutes with continued mixing at 7 Torr. Thereafter, 2 33 g of PURAC lactic acid preservative was added. The resulting solvent-free aqueous dispersion was milky white to light blue, which had a solids content of 35 wt%. Example 14 A prepolymer was prepared using a glove box in a dry nitrogen atmosphere. Filled in two separate 2000 ml Pyrex® glass reactors equipped with air pressure driven agitators, heating jackets and thermocouple temperature gauges, each filled with 44 〇 gram
Terathane 1800 — 醇(講自 Invista)及 440.0 克 Acclaim® 4220N(購自Bayer)。攪拌的同時將此二醇混合物加熱至5〇 °C ’隨後添加 150.0 克 Isonate® 125MDR(購自 DowTerathane 1800 - Alcohol (from Invista) and 440.0 g Acclaim® 4220N (available from Bayer). While stirring, the diol mixture was heated to 5 ° C. Then 150.0 g of Isonate® 125 MDR (purchased from Dow) was added.
Chemical)。然後持續攪拌的同時將該反應混合物加熱至9〇 C並維持在90°C下達120分鐘。將樣品自反應器取出,且 經測定分別含有2。/。NCO ’如藉由s. Siggia,"QuantitativeChemical). The reaction mixture was then heated to 9 ° C while continuing to stir and maintained at 90 ° C for 120 minutes. The sample was taken out of the reactor and determined to contain 2, respectively. /. NCO ’ by s. Siggia, "Quantitative
Organic Analysis via Functional Group",第三版,Wiley &Organic Analysis via Functional Group", Third Edition, Wiley &
Sons,New York’ 第 559-561 頁(1963)之方法所量測。 向3000毫升不銹鋼燒杯中填充1500克冷卻至約1〇〇c之超 純水、25.9克Bio-soft®N25-9及25·9克Stepantex®VT-90(二 者均購自Stepan公司)及10克Additive 65(購自Dow 123499.doc -36· 200907139 後用一具有轉子/定子混合頭之高剪切實驗室 ,100LC型)將此混合物以7〇〇〇 rpm混合3〇秒 在里。將如上於兩個反應器内製備之黏性預聚物倒至金屬管 狀圓筒中並藉助撓性管同時施力口空氣壓力%其添加至於水 溶液中之混合頭底部。預聚物溫度保持在介於5〇_7〇它之 間將、,里擠出之預聚物流分散並於700〇 rpm之持續混合下 用水再進行鏈延長2分鐘。此後添加2·33克puRAC®乳酸防Measured by the method of Sons, New York', pp. 559-561 (1963). Fill 3,000 cc of stainless steel beaker with 1500 g of ultrapure water cooled to approximately 1 〇〇c, 25.9 g of Bio-soft® N25-9 and 25.9 g of Stepantex® VT-90 (both from Stepan) Ten grams of Additive 65 (available from Dow 123499.doc -36. 200907139 followed by a high shear laboratory with a rotor/stator mixing head, Model 100LC) was mixed at 7 rpm for 3 sec. The viscous prepolymer prepared as described above in the two reactors was poured into a metal tubular cylinder and simultaneously applied to the bottom of the mixing head in the aqueous solution by means of a flexible tube simultaneously applying a port air pressure %. The prepolymer temperature was maintained between 5 Å and 7 Torr, and the extruded prepolymer stream was dispersed and continuously mixed at 700 rpm for 2 minutes with water. After that, add 2.33 grams of puRAC® lactate protection
腐劑。所得不含溶劑之水性分散液係乳白至淡藍色,其具 有35重量%之固體含量。 實例15-織物測試 本發明之組合物係與棉/LYCRA®織物(97%棉/3% lycra®氨綸)組合來測試。本實例之對照係用Uniii糟之 非濃縮C〇nfortTM織物軟化劑洗滌之織物。將表i中所示之 各組合物與棉/LYCRA®織物一起使用,藉由按照程序4於 4〇 °C下在Wascator®可編程自動洗滌機(得自Poisoning agent. The resulting solvent-free aqueous dispersion was milky white to light blue with a solids content of 35% by weight. Example 15 - Fabric Testing The compositions of the present invention were tested in combination with cotton/LYCRA® fabric (97% cotton/3% lycra® spandex). The control of this example was a fabric washed with Uniii's non-concentrated C〇nfortTM fabric softener. The compositions shown in Table i were used with cotton/LYCRA® fabrics in a Wascator® programmable automatic washer according to Procedure 4 at 4 °C.
Corning)。然 混合器(RossCorning). Mixer (Ross
Corp0ratlon,St〇ckh〇lm,Sweden)上使用標準負載織物達 2·5公斤負載進行洗滌。轉鼓乾燥之後,評價織物表面上 之任何沈積。三種織物皆未顯示出任何粉末或薄膜沈積。 表1中之組合物係如下: (a) 織物軟化劑(對照) (b) 織物軟化劑、1重量%實例6成膜陰離子聚胺基甲酸酯脲 之水为散液及2重量% Unimer(合成蠟以改良分散液) (C)織物軟化劑、1重量%實例5之聚胺基甲酸酯脲粉末、2 重置% Unimer(合成蠟以改良分散液)。 123499.doc •37- 200907139 處合包括織物軟化劑之細人私^ /& W <組合物(b)及(C)獲得一均句分散 液(無沉降及凝聚)。Washing was carried out on a Corp0ratlon, St〇ckh〇lm, Sweden) using a standard load fabric up to 2.5 kg load. After the drum was dried, any deposition on the surface of the fabric was evaluated. None of the three fabrics showed any powder or film deposition. The compositions in Table 1 are as follows: (a) fabric softener (control) (b) fabric softener, 1% by weight of Example 6 film-forming anionic polyurethane urea water as a dispersion and 2% by weight Unimer (Synthetic wax to improve the dispersion) (C) Fabric softener, 1% by weight of the polyurethane urethane powder of Example 5, 2 % by weight of Unimer (synthetic wax to improve the dispersion). 123499.doc •37- 200907139 The fine-grained fabrics including fabric softeners / / & W < compositions (b) and (C) obtained a uniform dispersion (no sedimentation and agglomeration).
對各織物之易護理性進行評價。熨烫之前及之後,使用 標準測試方法AATCC TM 124/IS〇 15487測定耐久㈣率 (DP率)。DP率得、織物三維光滑度之量度。熨斗滑動性 或易褽烫性係量測為使用角度約2〇。之褽烫板髮斗滑過織 & U所用之時間。易護理性結果展示於表1中。The ease of care of each fabric was evaluated. The durability (four) rate (DP rate) was determined before and after ironing using the standard test method AATCC TM 124/IS 〇 15487. The DP rate is a measure of the three-dimensional smoothness of the fabric. The slidability of the iron or the scalding is measured to an angle of about 2 inches. After the hot plate, the bucket is slid over the time used for weaving & U. The results of the easy care are shown in Table 1.
根據表1中之結果’其展示使用粉末或分散液處理之兩 種織物與對照(熨燙後增益〇 5點)相比均顯示更佳之率 改良(熨燙後增益丨點)。According to the results in Table 1 , it was shown that the two fabrics treated with the powder or dispersion showed a better rate of improvement (gain after ironing) compared to the control (gain after 5,000 points of ironing).
用本發明組合物處理之織物卬)及(c)亦顯示出熨斗在織 物表面上之更快滑動。 亦對組合物(a)、(b)、及⑷之香味/香氣實體化進行評 價。使二個人分別聞每一織物。此等人每一個均覺察到經 本發明組合物處理之經處理織物卬)及香氣更強烈。 亦對包括彼等經本發明組合物處理之織物的吸收特性 (濕氣處理)進行測試。量測此等特性以展示經本發明之粉 末或分散液處理後之織物與未處理織物相比之差異。 就上述織物⑷、(b)、及⑷之每-種而t,將亞麻油及 123499.doc -38- 200907139 水各一滴(約30微升)施 每-小滴所用時間並將其至完全吸收 織物完全吸收後__ ° ^中。亦量測經 記錄於表2中。 滴表面面積並以平方公分(cm2)The fabrics 卬) and (c) treated with the compositions of the present invention also show a faster sliding of the iron on the surface of the fabric. The aroma/aroma materialization of compositions (a), (b), and (4) was also evaluated. Let the two people smell each fabric separately. Each of these is aware that the treated fabric treated with the composition of the present invention has a stronger aroma. The absorption characteristics (moisture treatment) of the fabrics treated by the compositions of the present invention were also tested. These characteristics were measured to show the difference between the treated fabric of the powder or dispersion of the present invention compared to the untreated fabric. For each of the above fabrics (4), (b), and (4), t linseed oil and 123499.doc -38- 200907139 water each drop (about 30 microliters) per-droplet time and complete it The absorbent fabric is completely absorbed after __ ° ^. The measurement is also recorded in Table 2. Drop surface area in square centimeters (cm2)
戶斤T本發明之分散液⑻及粉末⑷在吸收方面較 對…、(a)有所改良。使用粉末形式⑷顯示顯著改良。 實例16-1〇〇%棉織物測試 亦對紅本發明組合物處理後之1G㈣棉織物進行測試。 此實例=對照係經濃縮之織物軟化劑(Colgate Palmoliva Softlan Ultra )。將表3中所展示之各組合物與ι〇〇〇/。棉織 物起使用,藉由按照程序4於40°C下在Wascator®可編程 自動洗務機(得自 Electr〇lux c〇rp〇rati〇n,St〇ckh〇im,The powder (8) and the powder (4) of the present invention are improved in terms of absorption compared to (a). A significant improvement was shown using the powder form (4). Example 16-1% Cotton Fabric Test 1G (four) cotton fabric treated with the red inventive composition was also tested. This example = Control Concentrated Fabric Softener (Colgate Palmoliva Softlan Ultra). Each of the compositions shown in Table 3 was mixed with ι〇〇〇/. Cotton fabrics are used by the Wascator® programmable automatic washing machine at 40 ° C according to Procedure 4 (available from Electr〇lux c〇rp〇rati〇n, St〇ckh〇im,
Sweden)上使用標準負載織物達2·5公斤負載進行洗滌。轉 豉乾燥之後,評價織物表面上之任何沈積。織物皆未顯示 出任何粉末或薄膜沈積。 表3中之組合物如下: (e) 織物軟化劑(對照) (f) 織物权化劑及1 0重量%實例1 〇之分散液、非離子聚胺基 123499.doc -39- 200907139 甲酸酯脲分散液 散液(無沉 結果展示 混5包括織物軟化劑之組合物⑺獲得均句分 降及凝聚)。量測各織物⑷及⑺之織 於表3中 + 表3 -織物伸長率Washing on a standard load fabric up to 2.5 kg load on Sweden). After the transfer drying, any deposition on the surface of the fabric was evaluated. None of the fabrics showed any powder or film deposition. The compositions in Table 3 are as follows: (e) Fabric softener (control) (f) Fabric righting agent and 10% by weight Example 1 Dispersion of liquid, nonionic polyamine group 123499.doc -39- 200907139 Formic acid The dispersion of the ester urea dispersion (the result of no sedimentation shows that the composition 5 comprising the fabric softener (7) obtains a uniform sentence drop and agglomeration). Measure the weave of each fabric (4) and (7) in Table 3 + Table 3 - Fabric elongation
較低增長值表明織物具有較佳恢復其起始形狀能力。 洗滌及沖洗循環後亦檢測織物⑷及⑺香味釋放之差 異。將1至2克各織物樣品置於—密封氣體取樣容器内。藉 由用剛滾珠軸承搖晃來施加織物應力。藉助τ_χΤΜ取樣 管使用氣體取樣幫浦以5G立方公分/分鐘運行2g分鐘將樣 品釋放之揮發性化合物自氣體取樣容器上部空隙抽出。該 TenexTM試管捕獲揮發性有機化合物(VOC)以作分析。缺後 以熱方式使TenexTM試管將揮發性有機物直接釋放至 GC/MSw作分析。表3a之VOC量測結果顯示自經含有實例 1〇之分散液(亦即,非離子聚胺基曱酸酯脲分散液)之織物 軟化劑沖洗之織物可釋放更多香味。 —— 表3a-V〇C測試 織物 揮發物濃度奈克/升/克 (e) 7 (f) l 48 123499.doc -40- 200907139 實例17 -氨論/棉接合織物測試 亦對經某些實施例之組合物處理後之氨綸/棉混紡機織 物進行測試。此實例之對照係經濃縮之織物軟化劑 (Colgate Palmolive 之 SoftlanTM Ultra)。將表4所示之各組 合物與氨論/棉混紡織物一起使用,藉由使用ArielTM液體 洗務劑於40°C按照程序4於4(TC下在Schutless®可編程自動 . 洗滌機上使用標準負載織物達2.5公斤負載洗滌並用18克 織物軟化劑組合物沖洗。轉鼓乾燥(於中等溫度下)後,評 價織物表面上之任何沈積。織物皆未顯示出任何粉末或薄 膜沈積。 表4中之組合物如下: (g) 僅經織物軟化劑處理之織物(對照) (h) 經織物軟化劑及1〇重量%之實例1〇之分散液(亦即,非 離子聚胺基甲酸酯脲分散液)處理之織物 此合包括織物軟化劑之組合物(11)獲得均句分散液(無沉 G $及凝聚)。量測各織物⑷及㈨之織物增長。結果展:於 表4中:A lower growth value indicates that the fabric has a better ability to recover its original shape. The difference in flavor release between fabrics (4) and (7) was also examined after washing and rinsing cycles. One to two grams of each fabric sample was placed in a sealed gas sampling container. The fabric stress is applied by shaking with a rigid ball bearing. The volatile compounds released from the sample were withdrawn from the upper space of the gas sampling vessel by means of a τ_χΤΜ sampling tube using a gas sampling pump operating at 5 g cubic centimeters per minute for 2 g minutes. The TenexTM tube captures volatile organic compounds (VOCs) for analysis. After the lack of heat, the TenexTM tube was used to release volatile organic compounds directly to the GC/MSw for analysis. The VOC measurement of Table 3a shows that the fabric softened by the fabric containing the dispersion of Example 1 (i.e., the nonionic polyamino phthalate urea dispersion) can release more fragrance. - Table 3a-V〇C test fabric volatiles concentration Nike / liter / gram (e) 7 (f) l 48 123499.doc -40- 200907139 Example 17 - ammonia theory / cotton joint fabric test also on some The spandex/cotton blended woven fabric treated with the composition of the examples was tested. The control for this example was a concentrated fabric softener (Colgate Palmolive's SoftlanTM Ultra). Each of the compositions shown in Table 4 was used with an ammonia/cotton blend fabric by using an ArielTM liquid detergent at 40 ° C according to Procedure 4 at 4 (using the Schutless® Programmable Automatic Washer). The standard load fabric was washed up to 2.5 kg load and rinsed with 18 grams of fabric softener composition. After drum drying (at moderate temperatures), any deposition on the fabric surface was evaluated. The fabric did not show any powder or film deposition. The composition is as follows: (g) fabric treated only with fabric softener (control) (h) fabric softener and 1% by weight of the dispersion of Example 1 (ie, nonionic polyurethane) Ester urea dispersion) treated fabric This composition comprises a fabric softener composition (11) to obtain a uniform dispersion (without sinking G $ and agglomeration). The fabric growth of each fabric (4) and (9) was measured. 4:
織物增長係一形狀伴 曰 ❿狀保持之里度。增長值代表 未恢復之伸县盎-y 、私你牙考期間 率。較低之增長值表明織物具有—較佳恢復 I23499.doc 200907139 其起始形狀之能力。 亦對兩種經某些實施例之组合物處理後之論/ 棉摻合織物進行測試。此實例之對照係經濃縮之織物軟化 #J (Colgate Palmolive^ Soupline^ Ultra) 〇 m^4a^4bm 示之各組合物與棉及LYCRA®氨綸摻合織物一起使用,藉 由使用得自Henkel C — on之Dixan®凝膠洗務劑於4〇υ 下按,、、、‘準程序在MleleTM市售洗務機上使用標準負載織 物達2.5 A斤負載洗滌並使用3〇毫升織物 洗1鼓乾燥(於中等溫度下)後,評價織物表面上:2 沈積。織物皆未顯示出任何粉末或薄膜沈積。對於下列織 物’ CK係一含95%棉_5% LYCRA®氨綸之圓型針織物且 wov係一含97%棉_3% LYCRA⑧氨綸之灰色緯向伸縮編織 物。 表4a及4b中之組合物如下: ⑴僅經織物軟化劑處理之織物(對照_ck) ω經織物軟化劑及丨〇重量%(3%活性組份)實例1〇之分散液 (亦即,非離子聚胺基甲酸酯脲分散液)處理之織物(經處 理-CK) (k)僅經織物軟化劑處理之織物(對照_w〇v) ⑴經織物軟化劑及10重量%(3%活性組份)之實例丨〇之分散 液(亦即,非離子型聚胺基曱酸酯脲分散液)處理之織物(經 處理-WOV) 123499.doc •42- 200907139 表4a-織物延長率CK 織物 增長%) (i)長度方向 7.5 (j)寬度方向 7.2 (i)長度方向 6.9 (j)寬度方向 6.4 表4b-織物延長率WOV 織物 增長(%) (k)緯向方向 7.29 (I)緯向方向 6.97 儘管已闡述目前據信為本發明之較佳實施例者,但熟悉 此項技術者應瞭解,可對其進行改變及修改而不背離本發 明之精神,且所有該等改變及修改均意欲包含於本發明之 實際範疇中。 123499.doc -43-The fabric grows in a shape with a ridge-like retention. The growth value represents the unrecovered rate of the county y-y, private period of your teeth. A lower growth value indicates that the fabric has the ability to recover its original shape, preferably I23499.doc 200907139. Two theories/cotton blend fabrics treated with the compositions of certain examples were also tested. The control of this example is a concentrated fabric softening #J (Colgate Palmolive^ Soupline^ Ultra) 〇m^4a^4bm each composition is used with cotton and LYCRA® spandex blend fabric, by using Henkel C — on the Dixan® gel cleaner under 4〇υ, , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , After drying (at moderate temperatures), the surface of the fabric was evaluated: 2 deposition. None of the fabrics showed any powder or film deposition. For the following fabrics 'CK' is a circular knit fabric containing 95% cotton _5% LYCRA® spandex and wov is a gray latitudinal stretch fabric containing 97% cotton _3% LYCRA8 spandex. The compositions in Tables 4a and 4b are as follows: (1) Fabric treated only with fabric softener (Control_ck) ω Fabric softener and 丨〇% by weight (3% active ingredient) Example 1 分散 dispersion (ie , Nonionic Polyurethane Urea Dispersion) Fabric Treated (Processed-CK) (k) Fabric treated only with fabric softener (Control_w〇v) (1) Fabric softener and 10% by weight ( 3% active ingredient) Example of a dispersion (ie, nonionic polyaminophthalate urea dispersion) treated fabric (treated - WOV) 123499.doc • 42- 200907139 Table 4a - Fabric Prolongation rate CK fabric growth %) (i) Length direction 7.5 (j) Width direction 7.2 (i) Length direction 6.9 (j) Width direction 6.4 Table 4b - Fabric elongation rate WOV Fabric growth (%) (k) Zonal direction 7.29 (I) The latitudinal direction of 6.97. While the present invention is believed to be a preferred embodiment of the present invention, those skilled in the art will appreciate that changes and modifications can be made without departing from the spirit of the invention, and all Variations and modifications are intended to be included in the actual scope of the invention. 123499.doc -43-
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