TW201406515A - 製備可流動性非晶型聚－α－烯烴黏著劑顆粒之方法 - Google Patents

製備可流動性非晶型聚－α－烯烴黏著劑顆粒之方法 Download PDF

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TW201406515A
TW201406515A TW102118481A TW102118481A TW201406515A TW 201406515 A TW201406515 A TW 201406515A TW 102118481 A TW102118481 A TW 102118481A TW 102118481 A TW102118481 A TW 102118481A TW 201406515 A TW201406515 A TW 201406515A
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adhesive
particles
fluid
temperature
pellets
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Darshak Desai
Yuhong Hu
Ken Gaspar
Ed Hantwerker
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Henkel Corp
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Abstract

本發明係關於一種製造自由流動性抗聚結非晶型聚-α-烯烴基黏著劑顆粒之方法。該方法包括(a)使該黏著劑擠壓通過浸沒於冷卻流體中之模板之孔口；(b)於該冷卻流體中將該黏著劑切割成複數個顆粒；(c)使該等顆粒在約25℃至約40℃之溫度範圍下固化至少30分鐘；及(d)自再結晶流體中分離出該等顆粒，並使該等顆粒乾燥。該等顆粒之硬化比以習知方式形成的顆粒快至少三倍。

Description

製備可流動性非晶型聚- α -烯烴黏著劑顆粒之方法
本發明係關於一種製造自由流動性抗聚結非晶型聚-α-烯烴基黏著劑顆粒之方法及由該方法製得之黏著劑顆粒。
熱熔性黏著劑通常係形成並包裝成固體塊，例如顆粒、白鰱狀物、枕狀物及塊狀物。固體塊係優於粉末，因為與裝載及卸載期間之吸入相關之風險較低，且具有與儲存及運送其等相關之便利性。亦希望該等黏著劑係以可儲存及隨後自動輸送並在應用位置饋入應用裝置中之形式提供。自由流動性抗聚結自由流動顆粒係有望減少終端操作者之中斷。
將柔軟及黏性塑膠材料製成顆粒之習知技術(如美國專利案第5,041,251號中所述)包括於冷卻流體中擠壓並切割該等材料，並使該等顆粒在該冷卻流體中保持至少若干小時至數天。自該冷卻流體中分離出該等顆粒並撒上蠟粉，以賦予不黏性。蠟通常具有高結晶度，且因而有助於自由流動。
非晶型聚-α-烯烴(APAO)基黏著劑具有低結晶度，內在柔軟並具有黏性，且傾向於在高溫下聚結(結塊)成巨大團塊。聚結黏著劑破壞終端操作，因為必須強行使聚結團塊再分散。為防止該聚結，通常將APAO基黏著劑包裝於鼓狀物中，或包裝成具有保護性包裝之個別白 鰱狀物、塊狀物及枕狀物；或在冷卻隔熱軌道車中運輸。由於以上限制，顆粒黏著劑通常係由高結晶度黏著劑(諸如乙烯醋酸乙烯酯)及高結晶度烯烴基黏著劑形成，而非由APAO基黏著劑形成。
此項技術中需要以抗聚結之快速產量生產非晶型聚-α-烯烴基黏著劑之顆粒。本發明滿足此需求。
本發明提供製備由非晶型聚-α-烯烴聚合物組成之抗聚結黏著劑顆粒之方法。該方法包括：(a)使該黏著劑擠壓通過浸沒於冷卻流體中之模板之孔口，該冷卻流體具有低於約45℉(7.2℃)之溫度T1；(b)於該冷卻流體中將該黏著劑切割成複數個顆粒；(c)使該等顆粒於再結晶流體(T2，其比T1高至少30℉)中固化至少30分鐘；及(d)自該再結晶流體中分離出該等顆粒，並使該等顆粒乾燥。
所得顆粒係自由流動且不結塊，且可在低於120℉之溫度下儲存及運輸很長時間而不聚結在一起。
本申請者已發現，使該等顆粒在約25至約40℃(77-104℉)之溫度範圍下再結晶可使黏著劑之再結晶速度自數天顯著提高至若干小時。本申請者亦已發現，所得顆粒之硬度特性比以習知方式形成的顆粒高至少三倍。
圖1A及1B係黏著劑之DSC掃描結果。
圖2係黏著劑顆粒在各種溫度下再結晶之動態時間掃描測試結果。
圖3顯示在各種溫度下再結晶之黏著劑顆粒之形變百分比。
本發明描述製備抗聚結顆粒之方法及由該方法製得之顆粒。該方法產生甚至在儲存及運輸高溫(亦即最高達120℉)下抗聚結之顆 粒。此外，該方法產生抗壓縮(其可導致黏結成巨大團塊)顆粒。
某些黏著劑組合物在儲存及運輸高溫(例如120℉)下具有聚結之傾向。該黏著劑組合物包含各種組分，且大多數係基於聚合物，諸如聚烯烴或苯乙烯嵌段共聚物，諸如SBS、SIS、SIBS及其摻合物。如本文所用，聚合物表示均聚物、共聚物、三聚物或互聚物。
該黏著劑中可使用任何具有冷結晶溫度之黏著劑，無論是結晶或是非晶型結構。該黏著劑較佳包含約30重量%至約90重量%的α-烯烴聚合物。在一實施例中，該聚合物係大於50%，較佳60%非晶形態。具有非晶形態之聚合物具有低結構有序度，且此種組織缺失導致無可見結晶度。在另一實施例中，該聚合物係大於30%，較佳50%半結晶形態。具有半結晶形態之聚合物係由結晶域及非晶域組成。較佳地，該半結晶聚合物包含小於30%的結晶度。
聚烯烴聚合物包括C2至C12共聚物。在一實施例中，聚烯烴共聚單體係由乙烯、丙烯、丁烯、己烯、4-甲基-1-戊烯及/或1-辛烯組成。示例性α-烯烴係選自由下列組成之群：乙烯、丁烯、戊烯-1、2-甲基戊烯-1、3-甲基丁烯-1、己烯-1、3-甲基戊烯-1、4-甲基戊烯-1、3,3-二甲基丁烯-1、庚烯-1、己烯-1、甲基己烯-1、二甲基戊烯-1、三甲基丁烯-1、乙基戊烯-1、辛烯-1、甲基戊烯-1、二甲基己烯-1、三甲基戊烯-1、乙基己烯-1、甲基乙基戊烯-1、二乙基丁烯-1、丙基戊烷-1、癸烯-1、甲基壬烯-1、壬烯-1、二甲基辛烯-1、三甲基庚烯-1、乙基辛烯-1、甲基乙基丁烯-1、二乙基己烯-1、十二碳烯-1及十六碳烯(hexadodecene)-1。
聚烯烴亦包括：高密度聚乙烯、低密度聚乙烯、極低密度聚乙烯、線性低密度聚乙烯或乙烯高碳數α-烯烴共聚物；聚丙烯，其包括柔軟聚丙烯、無規共聚物、衝擊共聚物或雜相聚丙烯及熱塑性硫化或TPV型聚丙烯；聚丁烯，其包括聚1-丁烯均聚物及共聚物或聚異丁 烯；辛烯、乙烯-丙烯單體或EPM、乙烯-丙烯-二烯單體或EPDM及其混合物。
示例性二烯共聚單體單元包括二乙烯基苯、1,4-己二烯、5- 1,6-辛二烯、5-甲基-1,4-己二烯、3,7-二甲基-1,6-辛二烯、1,3-環戊二烯、1,4-環己二烯及二環戊二烯。
在一較佳實施例中，該聚烯烴係乙烯、丙烯及丁烯之共聚單體。
該黏著劑另外包含其他組分，例如增黏劑。在一實施例中，基於該黏著劑之總重計，該黏著劑包含約10至約50重量%的增黏劑。示例性增黏劑包括天然及改質樹脂、多萜樹脂、苯酚改質烴樹脂、脂族及芳族烴樹脂、氫化烴、氫化樹脂及氫化樹脂酯及松香。松香及其衍生物之實例包括木松香、妥爾油、松脂、松脂膠、木松香、松香酯樹脂(包括其酯、氫化或去氫形式)；萜烯樹脂包括(例如)天然及合成萜烯、多萜烯及萜酯(terpenesters)；芳族或混合脂族-芳族增黏樹脂(如來自環戊二烯、二環戊二烯之聚合物)；苯乙烯樹脂，如來自苯乙烯、α-甲基苯乙烯、乙烯基甲苯、甲氧基苯乙烯、第三丁基苯乙烯、氯苯乙烯之共聚物；來自單體1,3-丁二烯、順式-1,3-戊二烯、反式-1,3-戊二烯、2-甲基-1,3-丁二烯、2-甲基-2-丁烯及其他可共聚單體之脂族樹脂或脂族石油烴樹脂。
較佳地，該增黏劑具有約80℃至150℃之軟化點(環球法(ring and ball method)，依據ASTM E28-58測量)。
視情況地，可將數量為0至約10重量%(以重量計)之蠟添加至該黏著劑中。該蠟可係天然或合成來源。適宜的天然蠟係植物蠟、動物蠟、地蠟或石化蠟。適宜的化學改質蠟係硬蠟，諸如褐煤酯蠟、沙索(sarsol)蠟等。適宜的合成蠟係聚伸烷基蠟及聚乙二醇蠟。較佳的蠟係石化蠟(諸如礦脂)、微蠟及合成蠟，特定言之為聚乙烯(PE)蠟、聚 丙烯(PP)蠟(視情況為PE或PP共聚物)、費托(Fischer-Tropsch)樹脂、石蠟或微晶蠟。
此外，可將最多約10重量%的增塑劑添加至該黏著劑中。適宜的增塑劑係藥用白油、環烷礦物油、鄰苯二甲酸酯、己二酸酯、聚丙烯、聚丁烯、聚異戊二烯寡聚物、氫化聚異戊二烯及/或聚丁二烯寡聚物、苯甲酸酯、植物或動物油及其衍生物。
該黏著劑可另外包含如下組分：諸如填充劑、抗氧化劑、佐劑、黏著促進劑、天然蠟、合成蠟、油、低分子量聚合物、結塊劑、抗結塊劑、顏料、加工助劑、UV安定劑、中和劑、潤滑劑、界面活性劑、成核劑、氧化聚烯烴、酸改質聚烯烴及/或酸酐改質聚烯烴。添加劑係作為個別組分、以母料形式或其組合與其他黏著劑組分組合。熟習此項技術者知道如何選擇及其性質。其等係以通常最多約3重量%及較佳約0.1至約2重量%之數量添加至該黏著劑中。
較佳地，該黏著劑係柔軟半壓感黏著劑，其具有以下針入度：(i)在25℃下處理1小時後為8至50dmm，(ii)在25℃下處理4小時後為10至45英寸/mm，(iii)在25℃下處理24小時後為10至40dmm。更佳地，該黏著劑具有以下針入度：(i)在25℃下處理1小時後為15至40dmm，(ii)在25℃下處理4小時後為15至40dmm，(iii)在25℃下處理24小時後為10至30dmm。
與高結晶度黏著劑不同，高APAO含量黏著劑在冷卻時不具有再結晶溫度。該等APAO基黏著劑具有冷結晶溫度，且任何具有冷結晶溫度之黏著劑均可用於所述方法中以形成不結塊的自由流動顆粒。雖然此項技術中已知各種測定冷結晶溫度(Tc)之方法，但本文所指出之Tc值係藉由差示掃描量熱儀(DSC)測定。首先將該黏著劑加熱至高於其熔化溫度以移除任何先前加熱史，然後冷卻至低於其玻璃轉變溫度(Tg)。APAO基黏著劑之緩慢結晶速度使該黏著劑在冷卻DSC掃描期 間維持非晶態。當在第二加熱DSC掃描中將該非晶型黏著劑緩慢加熱至高於其玻璃轉變溫度時，該黏著劑之非晶區域具有足夠動能及自由度以將其本身配置成結晶形式。該第二加熱掃描中所觀察到之放熱峰係測定為冷結晶溫度。雖然不受任何特定理論約束，但據信冷結晶提高該黏著劑之結晶度，且因此增加該黏著劑之硬度及強度。
在一較佳實施例中，該黏著劑之冷結晶溫度係在約82至約104℉(約28至約40℃)之範圍內。
用於製備抗聚結顆粒之方法包括使非晶型黏著劑在高溫下熔化，及然後於冷卻流體中將該黏著劑切割成複數個顆粒或立即浸沒於該冷卻流體中。可將該設備安裝成使得模板浸沒於該冷卻流體中或恰好位於該冷卻流體上方。在一實施例中，使該黏著劑擠壓通過直接位於該冷卻流體中之模板之孔口。
該冷卻流體具有低於約45℉(7.2℃)之第一溫度T1。下限值係取決於該流體，例如就水而言，該冷卻流體之下限值係約33℉(0.5℃)，且必須高於該冷卻流體之凝固點。該冷卻流體包括水、二醇、液態氮、壓縮二氧化碳等。當以充足量至少部份塗覆於顆粒表面上時，該冷卻流體可另外包括抑制顆粒結塊(亦即黏結、聚結、聚集及/或黏連)之抗結塊組合物。抗結塊組合物包括粉末、矽氧烷、界面活性劑、蠟、聚合物及其組合。
抗結塊組合物包括有機或無機化合物，諸如彼等選自由下列組成之群之化合物：滑石、雲母、碳酸鈣、微細或發煙矽石、有機酸、金屬有機酯、纖維素衍生物、氧化鋁三水合物、大理石粉、水泥塵、黏土、長石、氧化鋁、氧化鎂、氫氧化鎂、氧化銻、氧化鋅、硫酸鋇、矽酸鋁、矽酸鈣、二氧化鈦、鈦酸鹽、白堊、聚合物(諸如聚乙烯、聚丙烯、聚苯乙烯及其組合)。該等抗結塊組合物可以任何形式使用；然而，通常以粉末較佳。
通常，該等顆粒一經切割即運離孔口，以防止干擾連續擠壓/製粒過程。可藉由此項技術中已知之各種方法(例如，重力輸送、製程水流等等)將該等顆粒運離該孔口。如熟習此項技術者所知，根據製粒機之尺寸及速率，該製程水流在約35gpm至約350gpm之間變化。
然後使該等顆粒黏著劑於具有第二溫度T2之再結晶流體中再結晶/固化。該再結晶流體之溫度可視該黏著劑而變化。在一實施例中，該再結晶流體具有約77至約105℉(約25℃至約41℃)之T2範圍。在一較佳實施例中，再結晶流體具有約82至約104℉(約28℃至約40℃)之T2範圍。
與使該等顆粒之總體溫度驟變或降低以迫使再結晶之習知技術相反，本發明方法使該等顆粒曝露至較高再結晶溫度下以加速固化過程。在較佳方法中，該等顆粒係在具有指定T2之再結晶流體中停留最少約30分鐘，較佳至少100分鐘。
該等顆粒在該再結晶流體中係以比習知方法快至少三倍之速度硬化及再結晶，且該等顆粒在該再結晶流體中約40(較佳120)分鐘後具有足夠硬度或足夠低形變。
該再結晶流體包括水、二醇、液態氮、壓縮二氧化碳等。該再結晶流體亦可包括抗結塊組合物。
然後自該再結晶流體中分離出該等再結晶顆粒，並使其乾燥。乾燥後，視情況將乾燥抗結塊組合物撒佈及塗覆在該等再結晶顆粒上。
該等顆粒之形狀可根據製造方法而有所不同。其等可具有小型枕狀物之形式，較佳球形(如球體)，或在另一較佳實施例中，其等形成圓柱形。在此情況下，各方向上之尺寸係不同，例如在一個方向上為25mm，且直徑為2至10mm。該等顆粒之形式不必要係規則，例如，球形可經壓縮或拉伸，棒狀可係對稱或具有不規則形式，只要該 等顆粒之尺寸不過大即可。該形式將受製造方法影響，例如該等顆粒係經擠壓、切割及分離以得到不完全圓形。可混合不同形式及尺寸之顆粒，但此並非較佳。本發明之另一態樣係關於該等顆粒之尺寸。在一實施例中，該等顆粒各具有大於約5mg且小於約200mg，較佳小於約100mg，最佳小於約80mg之重量。較小粒度可提升材料之流動性質。
一般而言，以習知方式製造之主要包含非晶型或半結晶形態之聚合物通常產生柔軟顆粒。該等柔軟顆粒在長期儲存及高溫時係傾向於聚結。根據本發明之顆粒在最高達120℃之溫度下顯示自由流動性。該自由流動性在高溫儲存後亦保持穩定。
雖然習知方法將顆粒保存在冷卻流體中以迫使再結晶，但本發明方法使該等顆粒在比該冷卻流體高至少30℉之溫度下固化。出乎意料的是，本發明方法使黏著劑之固化速度增加至少3倍。此外，即使僅在再結晶進行約120分鐘後，該等由本發明方法製得之黏著劑顆粒仍具有比由習知方法製得之顆粒低至少三倍之形變百分比值。
提供以下實例以更詳細地描述本發明。此等闡述當前用於實施本發明之較佳模式之實例係意欲說明而非限制本發明。
實例
實例1：黏著劑之針入度
在25℃下以各種時間處理黏著劑樣品，且然後依據ASTM D1321以針入度儀測量針入度值。表1顯示結果。
*1dmm=0.1mm
樣品A、B及C之針入度值係高於比較樣品D及E，此表明樣品A、B及C係比較堅硬的比較樣品D及E柔軟。比較樣品D及E由於其低針入度值而可易於製成顆粒。在此項技術中通常應理解：較柔軟或半壓感黏著劑係更難以製成不結塊顆粒。
實例2：測定峰值再結晶溫度
藉由差示掃描量熱儀(DSC)測定該等黏著劑之冷結晶溫度，並匯總於表2中。使各黏著劑以10℃/min熔化至180℃，然後以10℃/min冷卻至-50℃，並在-50℃下維持10分鐘。然後以3℃/min對該黏著劑再加熱，直至180℃。使用DSC Universal V4.5A TA Instrument軟體，將冷結晶峰(Tc)測定為該第二DSC加熱之峰值放熱溫度。
樣品A及樣品E之冷卻及第二加熱合成曲線係分別顯示於圖1A及1B中。樣品A、B及C在冷卻期間不具有再結晶溫度(Tr)。只有在第二加熱時，樣品A、B及C才顯示冷結晶溫度。與樣品A、B及C不同，比較樣品D及E在冷卻時快速再結晶。
實例3
藉由試產級製粒機，按照以下製程生產黏著劑顆粒：
1.將APAO基黏著劑(具有>50%聚丙烯-聚丁烯共聚物之APAO黏 著劑)裝載於攪拌加熱式混合槽中，並使其在175℃下熔化。
2.迫使該熔融黏著劑通過孔口(尺寸2.8mm)，並於冷卻水流中切割。該冷卻水流包含水T1(4℃)，並以約55至約65gpm之流速使該等顆粒向下游移動。冷卻槽亦包含1.0%抗結塊劑。該等顆粒流入攪拌式再結晶/固化槽中。
3.該攪拌式再結晶/固化槽包含水及0.1%抗結塊劑。將該再結晶/固化槽之溫度設定為T2(35℃)。
4.使該等顆粒於該再結晶/固化槽中停留約120分鐘。
實例4：動態時間掃描測試
測試顆粒在各種T2溫度下再結晶/固化之時間掃描曲線。針對各顆粒樣品運行ARES M中之動態時間掃描程式。在施用溫度(150℃)下，於兩塊平行板之間加熱該等顆粒樣品，並使其迅速冷卻至指定再結晶/固化溫度(40、80、85、90、100或105℉)，並保持24小時(hr)。以1.0%之等應變施加10rad/sec之頻率，並經時記錄模量。圖2顯示針對時間之Tan δ值。Tan δ=1時之溫度描繪該黏著劑由液體變成固體之轉折點(大於Tan δ=1之值描繪液體狀黏著劑，而小於Tan δ=1之值描繪固體狀黏著劑)。
如圖2中所示，在習知再結晶溫度(40℉)下使該等顆粒再結晶需要明顯更長的時間方能穿過Tan δ=1之值，而在90℉下使該等顆粒固化使固化速率提高至少3倍。另外，當該等顆粒在90℃下再結晶時，該等顆粒係比習知方法顯著更快地固化。
實例5：時間溫度掃描測試中達到Tan δ=1之滯留時間
根據該時間溫度掃描測試，將達到Tan δ=1所經歷之滯留時間匯總於表3中。
如表3中所示，使樣品A於80℉或以上之溫度下固化使得達到Tan δ=1之保持時間減少至少20%。此外，將T2提升至高於85℉且低於150℉使固化過程之速度最大化。
實例6：形變/硬度
藉由測量在各種T2流體溫度下固化之顆粒之形變百分比來檢測樣品A顆粒的硬度。藉由以改良的測微計(具有磁鐵及鋼)測量初始直徑(d0)來檢測顆粒形變。將70g之重量置於該顆粒上一分鐘，然後測量新直徑(d1)。計算至少十二個顆粒樣品之差異百分比((d0-d1)/d0 x 100%)，並在圖3中顯示相對於再結晶流體溫度之形變百分比。
圖3顯示：當該等顆粒在85℉及90℉之T2下固化時，平均形變係最小。在90℉下固化之顆粒即使僅在約40分鐘後仍實現低於約30%之形變。事實上，當於90℉下再結晶時，大多數顆粒僅在約40分鐘後便實現低於約20%之形變。相反地，即使在再結晶進行超過60分鐘時，在48℉至76℉之溫度下固化之顆粒仍具有約60至約80%之形變範圍。
另外，如圖3中所示，該等顆粒在85℉及90℉下之固化係比在較低溫度範圍下之固化明顯更快，且形變更小。
實例7：結塊性
藉由將約950g重量均勻分佈於約200g由在各種溫度下固化之樣品A製成之顆粒之頂部來測量結塊性。然後將整個裝置轉移至120℉烘箱中並保持24小時。然後將該裝置移出，並冷卻至室溫(約20℃)。 然後以肉眼及手工方式觀察該等顆粒。若該黏著劑結成塊，則評定為「不合格」；且將完全不結塊的黏著劑評定為「合格」。
如熟習此項技術者所瞭解，可在不脫離本發明之精神及範圍下對其作出許多修改及變化。本文所述之具體實施例僅係僅作為實例而提供，且本發明係欲僅受隨附申請專利範圍之條款及此等申請專利範圍所有權具有之等效物之完整範圍限制。

Claims (10)

  1. 一種形成複數個黏著劑顆粒之方法，其包括以下步驟：a)使該黏著劑擠壓通過浸沒於冷卻流體中之模板之孔口，該冷卻流體具有T1之溫度；b)於該冷卻流體中將該黏著劑切割成複數個顆粒；c)使該等顆粒在T2之再結晶流體中固化至少30分鐘；d)自該再結晶流體中分離出該等顆粒，並使該等顆粒乾燥，其中該T1係低於約45℉(7.2℃)，且該T2比T1高至少30℉。
  2. 如請求項1之方法，其中該T2具有約25℃至約40℃(約77℉至約104℉)之溫度範圍。
  3. 如請求項1之方法，其中使該等顆粒在該再結晶流體中保持至少約60分鐘至約180分鐘。
  4. 如請求項1之方法，其中該黏著劑係熱熔性黏著劑。
  5. 如請求項1之方法，其中該非晶型α-烯烴聚合物包含乙烯、丙烯、丁烯、戊烯、己烯、庚烯、辛烯、壬烯、癸烯、十一碳烯、十二碳烯及其混合物之共聚單體。
  6. 如請求項1之方法，其中該非晶型α-烯烴聚合物包含丙烯及丁烯共聚單體。
  7. 如請求項1之方法，其中該熱熔性黏著劑具有以下針入度：(i)在25℃下處理1小時後為8至50dmm，(ii)在25℃下處理4小時後為10至45dmm，(iii)在25℃下處理24小時後為10至40dmm。
  8. 如請求項1之方法，其中該熱熔性黏著劑具有約77至約105℉(約25至約41℃)之冷結晶溫度。
  9. 一種物件，其係藉由如請求項1之方法製得。
  10. 如請求項9之物件，其中該等顆粒具有低於40%之平均形變百分 比；其中該形變百分比係(d0-d1)/d0 x 100%，d0係初始直徑，且d1係在施加70g之重量一分鐘後所測得之直徑。
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