TWI494396B - 可分散非織物 - Google Patents

可分散非織物 Download PDF

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TWI494396B
TWI494396B TW102111106A TW102111106A TWI494396B TW I494396 B TWI494396 B TW I494396B TW 102111106 A TW102111106 A TW 102111106A TW 102111106 A TW102111106 A TW 102111106A TW I494396 B TWI494396 B TW I494396B
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woven
weight
aqueous medium
emulsion polymer
dispersible
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Paul Nedwick
Katherine Sue Rice
Maureen B Nunn
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Rohm & Haas
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Description

可分散非織物
本發明係關於一種形成可分散非織物基材的方法。更詳而言，本發明係關於在水性介質中形成可分散非織物基材的方法，係包括：a)形成包括乳劑聚合物的水性非織物黏合劑，該聚合物係包括下述作為共聚單元，以該乳劑聚合物之重量為基準計，10wt%至30wt%之單乙烯系不飽和單酸單體，其中，乳劑聚合物之Tg係-20℃至30℃；其中，聚合物業經包含三經取代之N原子的化合物修飾，該化合物係具有4至7的pKb ；b)使非織物基材與水性非織物黏合劑接觸；c)將經接觸之非織物加熱至120℃至220℃之溫度；以及d)將經接觸及加熱之非織物浸潤於具有最終pH<5之水性介質中，以於水性介質中提供可分散非織物。亦提供一種藉由前述方法於水性介質中所形成之可分散非織物基材，及一種於水性介質中提供經分散之非織物的方法。
美國專利案第5,451,432號揭露一種使用水載型不含甲醛之組成物處理撓性及多孔基材的方法，該組成物係含有某些共聚合之乙烯系不飽和二羧酸或其衍生 物，其中黏合劑係以固定鹼部份地中和之。將經處理之非織物基材分散之前，經處理之非織物基材的可分散性與維持所欲水準之濕強度兩者之間的改良平衡仍為所期望。業發現本發明提供該等所欲之特性。
於本發明之第一態樣中，係提供一種於水性介質中形成可分散非織物基材之方法，係包含：a)形成包含乳劑聚合物的水性非織物黏合劑，聚合物係包含下述作為共聚單元，以乳劑聚合物之重量為基準計，10wt%至30wt%之單乙烯系不飽和單酸單體，其中，該乳劑聚合物之Tg係-20℃至30℃；其中，該聚合物業經包含三經取代之N原子的化合物修飾，該化合物係具有自4至7的pKb ；b)使非織物基材與該水性非織物黏合劑接觸；c)將經接觸之非織物加熱至120℃至220℃之溫度；以及，d)將經接觸及加熱之該非織物浸潤於具有最終pH<5之水性介質中，以提供可分散非織物於水性介質中。
於本發明之第二態樣中，係提供一種於水性介質中提供經分散之非織物的方法，係包含將申請專利範圍第1項或第2項之可分散非織物浸潤於過量之pH>6.5的水性介質中。
於本發明之第三態樣中，係提供一種於水性介質中之可分散非織物，係藉由本發明之第一態樣之方法形成。
於本發明之形成於水性介質中之可分散非織物基材的方法中，本文中之「水性」係意指一種組成物，其中連續相為水，或者為包含主要為水但亦視需要包括水可溶混之溶劑的混合物。本文中之「可分散」係意指，於適宜之條件下，非織物基材可被導致瓦解為下述之至少一者：較小之碎片、纖維之凝集體、獨立之纖維、及其混合物。
本文中之「非織物」係意指纖維之類織物組合體，典型係呈片狀或網狀形式，其並非為經編織或針織之材質。非織物基材係包括紙張；非織織物；氈及墊；或其他纖維之組合體。非織物基材可包括：纖維素纖維如棉、人造絲及木漿；合成纖維如聚酯、玻璃及尼龍；雙成份纖維；及其混合物。較佳為占支配量的能參與氫鍵鍵結的纖維。更佳係包括占支配量的纖維素纖維的非織物基材。非織物基材可藉由發明所屬技術領域中習知之方法如，舉例而言，濕式佈層、氣流佈層、網狀結合及水刺成網法而形成。纖維典型係經選擇，俾使其長度及組成不危害經處理之非織物基材的最終可分散性。
於本發明之在水性介質中形成可分散非織物基材的方法中，係形成水性非織物黏合劑，黏合劑係包括乳劑聚合物，該乳劑聚合物係包括下述作為共聚單元，以乳劑聚合物之重量為基準計，10wt%至30wt%之單乙烯 系不飽和單酸單體，其中，乳劑聚合物之Tg(藉由福克斯方程式(Fox equation)計算之玻璃轉化溫度)係-20℃至30℃；其中，聚合物業經包含三經取代之N原子的化合物修飾，該化合物係具有4至7的pKb 。本文中之「黏合劑」係意指包括聚合物之組成物。
水性非織物黏合劑係包括乳劑聚合物；亦即，藉由乙烯系不飽和單體於水性乳劑聚合製程中之加成聚合而製備的聚合物。乳劑聚合物可係可固化者，亦即，其可於施以能量，最典型為加熱之情況下，進行某種程度之化學製程，例如形成共價鍵。乳劑聚合物係包括下述作為共聚單元，以乳劑聚合物之重量為基準計，10wt%至30wt%，較佳12wt%至25wt%之單乙烯系不飽和單酸單體。單酸單體係包括，舉例而言，羧酸類單體如，舉例而言，丙烯酸、甲基丙烯酸、巴豆酸、伊康酸單甲酯、富馬酸單甲酯、富馬酸單丁酯。較佳係丙烯酸。
乳劑聚合物視需要包括下述作為共聚單元，以乳劑聚合物之重量為基準計，0.01wt%至0.75wt%，較佳自0.2wt%至0.6wt%之單乙烯系不飽和二羧酸單體如，舉例而言，伊康酸、富馬酸、馬來酸；包括其酐、鹽、及其混合物。較佳係伊康酸。
乳劑聚合物除了經共聚之單酸以及視需要之二羧酸單體之外，亦包括至少一種其他共聚之乙烯系不飽和單體如，舉例而言，(甲基)丙烯酸酯單體，包括(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丁酯、(甲 基)丙烯酸2-乙基己酯、(甲基)丙烯酸癸酯、(甲基)丙烯酸羥乙酯、(甲基)丙烯酸羥丙酯、脲基官能性(甲基)丙烯酸酯類及(甲基)丙烯酸之乙醯乙酸酯類、乙醯胺類或氰基乙酸酯類；苯乙烯或經取代之苯乙烯；乙烯基甲苯；丁二烯；醋酸乙烯酯或其他乙烯基酯類；乙烯基單體如氯乙烯、偏氯乙烯；以及(甲基)丙烯腈。較佳係丙烯酸乙酯。如貫穿本揭露所使用者，後附另一術語之術語「(甲基)」如(甲基)丙烯酸酯或(甲基)丙烯醯胺，係分別指丙烯酸酯類與甲基丙烯酸酯類兩者或丙烯醯胺類與甲基丙烯醯胺類兩者。較佳係不包括可於聚合時或後續加工過程中產生甲醛之單體如，舉例而言，N-羥烷基(甲基)丙烯醯胺(N-alkylol(meth)acrylamide)。選擇至少一種其他經共聚之乙烯系不飽和單體，使乳劑聚合物將具有所需要範圍內之Tg。
於某些具體實施例中，乳劑聚合物可包括，以聚合物之重量為基準計，0至2wt%，或0至0.1wt%之經共聚之多乙烯系不飽和單體，但必須選擇其量，以不會在本質上傷害經包括乳劑聚合物之水性非織物黏合劑處理之非織物基材的可分散性。多乙烯系不飽和單體係包括，舉例而言，(甲基)丙烯酸烯丙酯、鄰苯二甲酸二烯丙酯、1,4-丁二醇二(甲基)丙烯酸酯、1,2-乙二醇二(甲基)丙烯酸酯、1,6-己二醇二(甲基)丙烯酸酯、及二乙烯基苯。
亦設想具有不同組成之乳劑聚合物的混合物。對於兩種或更多種乳劑聚合物之混合物，其經共聚之單酸及選擇性之二羧酸含量以及Tg應取決於乳劑聚合物 之整體組成，而不考慮其內之乳劑聚合物的數目或個別組成。
用以製備乳劑聚合物之乳劑聚合技術係發明所屬技術領域中所習知如，例如美國專利案第4,325,856號、第4,654,397號及第4,814,373號中之揭示。可使用習知界面活性劑如，舉例而言，陰離子性及/或非離子性乳化劑如，舉例而言，烷基硫酸之銨或鹼金屬鹽類、烷基磺酸類、脂肪酸類、可共聚之界面活性劑及氧乙基化烷基酚類。較佳係陰離子乳化劑。所使用之界面活性劑的量通常為，以總單體之重量為基準計，0.1wt%至6wt%。可使用熱起始製程或氧化還原起始製程。可使用習知之自由基起始劑如，舉例而言，過氧化氫、氫過氧化第三丁基、氫過氧化第三戊基、過硫酸銨及/或鹼性過硫酸鹽基，其用量典型為，以總單體之重量為基準計，0.01wt%至3.0wt%。可以類似的量使用氧化還原系統，該氧化還原系統使用相同的起始劑，配合使用適當之還原劑，舉例而言，甲醛次硫酸鈉、亞硫酸氫鈉、異抗壞血酸、硫酸羥胺及亞硫酸氫鈉，視需要可結合使用金屬離子，舉例而言，鐵及銅，視需要復包含用於金屬之錯合劑。可使用鏈轉移劑如硫醇以降低聚合物之分子量。單體混合物可以純淨物加入或作為水乳劑加入。單體混合物可以單一組成或可變組成，以一次性加入或多次加入，或於反應期間連續加入。額外的組成分可加入於反應前、反應中，或後續之任何階段，舉例而言，自由基起始劑、氧化劑、還原劑、鏈轉移劑、中和劑、界 面活性劑及分散劑。可採用獲得多峰粒徑分佈之製程如，舉例而言，於美國專利案第4,384,056號及第4,539,361號中揭示之彼等。
於本發明之另一具體實施例中，乳劑聚合物可藉由多階乳劑聚合製程製備之，其中，至少兩個具有不同組成之階段係依序聚合。此製程導致至少兩種互不相容之聚合物組成的形成，由是導致在聚合物顆粒中形成至少兩相態。此等顆粒係由具有不同幾何形狀之兩相或更多相組成如，舉例而言，核/殼或核/鞘顆粒、殼相不完全封裝核之核/殼顆粒、多重核之核/殼顆粒、以及互插之網狀顆粒。此等多階乳劑聚合物之每一階段可含有選自本文前示之用於乳劑聚合物之彼等的單體、界面活性劑、鏈轉移劑等。對於多階乳劑聚合物，經共聚之單酸及二羧酸含量及Tg應自乳劑聚合物之整體組成而決定，而不考量其內之階或相的數目。用以製備此等多階乳劑聚合物之聚合技術係發明所屬技術領域中習知者如，舉例而言，美國專利案第4,325,856號、第4,654,397號及第4,814,373號。
乳劑聚合物之玻璃轉化溫度(Tg)的計算值為-20℃至30℃。本文中，聚合物之Tg係使用福克斯方程式(T.G.Fox,Bull.Am.Physics Soc.,Volume 1,Issue No.3,p.123(1956))所計算之彼等。亦即，舉例而言，為了計算單體M1與M2之共聚物的Tg，1/Tg(計算值)=w(M1)/Tg(M1)+w(M2)/Tg(M2)，其中，Tg(計算值)係針對共聚物計算之玻璃轉化溫度
w(M1)係共聚物中單體M1之重量分率
w(M2)係共聚物中單體M2之重量分率
Tg(M1)係M1之均聚物的玻璃轉化溫度
Tg(M2)係M2之均聚物的玻璃轉化溫度，全部溫度之單位為°K。
均聚物之玻璃轉化溫度可於，舉例而言，《聚合物手冊》(Polymer Handbook,J.Brandrup and E.H.Immergut,Interscience Publishers)中找到。在任何條件下，於下列聚酸之福克斯方程式計算中，皆使用下述之均聚物Tg：聚(甲基丙烯酸)Tg=185℃；聚(丙烯酸)Tg=106℃；聚(伊康酸)Tg=154℃；以及聚(馬來酸酐)Tg=154℃。
乳劑聚合物顆粒之平均顆粒直徑典型係30奈米至500奈米，較佳係200奈米至400奈米，其係藉由布魯克海文儀器公司(Brookhaven Instrument Corp.,Holtsville,NY)提供之布魯克海文BI-90型粒度儀測量者。
本發明之水性非織物黏合劑較佳係不含甲醛之組成物。本文中，「不含甲醛之組成物」係意指組成物實質上不含甲醛，亦不會因為乾燥及/或固化而實質性釋放甲醛。為了將組成物中之甲醛含量減至最低，較佳係於製備本發明之乳劑聚合物時，使用聚合佐劑如，舉例而言，起始劑、還原劑、鏈轉移劑、殺生物劑、界面活性劑等，該等佐劑係本身不含甲醛、在聚合製程中不產生甲醛且在基材處理過程中不產生或釋放甲醛。當水性組成物中可接受低量之甲醛時，或當存在使用產生或釋放甲醛之佐劑的 強制原因時，可使用此等組成物。
乳劑聚合物係以包括三經取代之N原子的化合物修飾，該化合物係具有自4至7之pKb 。該pKb係藉由習知方法於20℃於水中測定。亦設想包括三經取代之N原子的聚合性材質，可使用具有4至7之pKb 的化合物。化合物係包括，舉例而言，單乙醇胺、二乙醇胺及三乙醇胺、聚乙烯基吡咯烷酮、阿拉伯膠、醯胺化果膠、聚葡萄胺糖、明膠、阿拉伯膠。較佳之化合物係單乙醇胺、二乙醇胺及三乙醇胺。該修飾可於接觸非織物基材之後續步驟之前、過程中或之後但於加熱經接觸之非織物的步驟之前產生效應。以包括三經取代之N原子之化合物修飾的程度，以當量為基準中和乳劑聚合物之酸基，典型為1%至120%之範圍，較佳25%至110%，更佳75%至105%，且最佳95%至105%，其中，該化合物係具有4至7之pKb 。
水性非織物黏合劑除了包括乳劑聚合物之外，亦可包括習知之處理成份如，舉例而言，乳化劑、顏料、填充劑或擴展劑、抗遷移酸、固化劑、聚結劑、界面活性劑、殺生物劑、塑化劑、有機矽烷、抗發泡劑、腐蝕抑製劑、著色劑、蠟、其他聚合物、及抗氧化劑。
於本發明之在水性介質中形成可分散非織物基材的方法中，非織物基材係與水性非織物黏合劑接觸。典型地，以乾燥重量為基準計，非織物黏合劑與所接觸之非織物基材的非織物黏合劑之比率以百分比表達，亦稱為%添加，係1%至25%，較佳係1%至10%，其選擇係取 決於非織物基材之強度及所欲之最終用途。使用習知應用技術如，舉例而言，空氣噴灑或無空氣噴灑、填塞、浸透、輥塗、簾塗、凹版印刷等將非織物基材與水性非織物黏合劑接觸。非織物基材可與水性非織物黏合劑接觸，以在接近一個或兩個表面處提供黏合劑，或將黏合劑貫穿結構而均勻或不均勻分佈。亦設想，當所欲者係圖案化分佈時，可以非均勻手段將水性非織物黏合劑施用至一個或兩個表面。
於本發明之在水性介質中形成可分散非織物基材的方法中，將業經與水性非織物黏合劑接觸之非織物基材加熱至120℃至220℃，較佳140℃至180℃之溫度，加熱時間係足以達成可接受水準之乾燥及/或固化。若需要，乾燥及固化功能可於兩個或更多個不同之步驟中產生效應。舉例而言，可首先於一溫度將組成物加熱一段時間，足以將其實質上乾燥但不足以將組成物實質上固化，隨後，於更高溫度加熱第二段時間及/或更長時間以產生固化效應。此過程，指為「B-分段」，可用以提供經黏合劑處理之例如呈卷形式之非織物，其可於遲些時候被固化，與固化製程同時，可形成或不形成或者模鑄或不模鑄為特定構型。
於本發明之在水性介質中形成可分散非織物基材的方法中，將經接觸且加熱之非織物基材浸潤於具有最終pH<5，較佳最終pH為3.0至4.99的水性介質中，以提供可分散非織物於水性介質中。本文中，「最終pH」 係意指經接觸且加熱之非織物浸潤於其中之水性介質的pH(於20℃測量)。若使用所選擇之非織物與水性介質及其量未達成最終pH<5，係於浸潤步驟之前、期間或之後，藉由加入酸性材質如，舉例而言，檸檬酸而將pH調節至所欲之範圍。咸信，水性介質所需要之pH係對經加熱處理之非織物的濕強度有有利貢獻，且對於某些經熱處理之非織物可存儲於其中的組成物如，舉例而言，擦洗溶液及洗滌液而言，該pH亦係適宜之pH。典型地，水性介質之重量係經接觸且加熱之非織物基材的0.1至10倍，較佳0.5至5倍。
於本發明於水性介質中提供可分散非織物的方法中，係將本發明可分散非織物浸潤於pH>6.5，較佳係最終pH>6.5，較佳係最終pH為6.8至10.0的過量水性介質中。本文中，「過量水性介質」係意指水性介質之重量係大於經接觸且加熱之非織物的重量。於制定之pH(於20℃測量)，經加熱處理之非織物的濕強度顯著降低，以促進其瓦解為下列之至少一者：較小之碎片、纖維之凝集體、獨立之纖維、及其混合物。當然，可施用之任意機械力將輔助此分散製程如，舉例而言，若經處理非織物係沉積於pH>6.5之過量水中且經受剪切力如沖馬桶之動作。
本文中，於水性介質中之可分散非織物係藉由本發明之在水性介質中形成可分散非織物的方法所形成者。
所使用之縮寫
AA=丙烯酸
EA=丙烯酸乙酯
IA=伊康酸
MMA=甲基丙烯酸甲酯
Sty=苯乙烯
DI水=去離子水
測試方法： 所使用之乳劑聚合物：(以重量為基準計之組成)
乳劑聚合物A=p(84 EA/1 Sty/15 AA)
乳劑聚合物B=p(84 EA/1 Sty/14.5 AA/0.5 IA)
乳劑聚合物C=p(59 EA/1 Sty/20 MMA/19.5 AA/0.5 IA)
實施例1至6及比較例A及B.可分散非織物之形成及評估
製備下述水性非織物黏合劑。加入次序為水、胺，混合直至溶解；隨後於混合下加入乳劑聚合物。
對於每一樣本，秤重兩片Whatman 4號濾紙。Whatman 4號濾紙係使用博馳兄弟軋車(Birch Brothers Padder(Birch Brothers Southern,Inc.))於35psi壓力下以設定為5之速率予以浸漬及充填；並於150℃加熱3分鐘。將經處理之紙再次秤重並使用下列方程式計算添加：%添加=(最終重量-起始重量)*100%/最終重量
可分散非織物之評估
將乳劑聚合物A塗覆於Whatman 4號濾紙上。將9條1吋x 4吋條帶CD於50g商用水性洗滌液A中浸泡30分鐘，再於業經使用110ppm碳酸氫鈉將其調節為pH=7的0.1wt% TRITONTM X-100(陶氏化學公司(The Dow Chemical Company)之產品)自來水中浸泡，測量拉伸強度(9次測試之平均值)。
實施例1至3，本發明之可分散非織物基材於pH<5顯現提升之拉伸強度，且於pH>6.5顯現下降之拉伸強度，顯示非織物的可分散性，相較於未修飾之乳劑聚合物(比較例A)，其於指定pH範圍內無顯著之拉伸強度變化。
實施例4至6，本發明之可分散非織物基材於pH<5顯現提升之拉伸強度，於pH>6.5顯現下降之拉伸強度，顯示非織物的可分散性，相較於未修飾之乳劑聚合物(比較例B)，其於指定pH範圍內無顯著之拉伸強度變化。

Claims (4)

  1. 一種於水性介質中形成可分散非織物基材之方法，係包含：a)形成包含乳劑聚合物的水性非織物黏合劑，該聚合物係包含下述作為共聚單元，以該乳劑聚合物之重量為基準計，10wt%至30wt%之單乙烯系不飽和單酸單體，其中，該乳劑聚合物之Tg係-20℃至30℃；其中，該聚合物業經包含三經取代之N原子的化合物修飾，該化合物係具有4至7的pKb ；b)使非織物基材與該水性非織物黏合劑接觸；c)將該經接觸之非織物加熱至120℃至220℃之溫度；以及d)將經接觸及加熱之該非織物浸潤於具有最終pH<5之水性介質中，以提供可分散非織物於水性介質中。
  2. 如申請專利範圍第1項之於水性介質中提供該可分散非織物基材的方法，其中，該乳劑聚合物復包含以該乳劑聚合物之重量為基準計，0.01wt%至0.75wt%之單乙烯系不飽和二羧酸單體作為共聚單元。
  3. 一種於水性介質中提供經分散之非織物的方法，係包含將如申請專利範圍第1項或第2項之可分散非織物浸潤於過量之pH>6.5的水性介質中。
  4. 一種於水性介質中之可分散非織物，係藉由申請專利範圍第1項或第2項之方法形成。
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