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TW202246402A - 1,4-雙(2-乙基己基)環己烷二甲酸酯在表面覆蓋物中作為增塑劑的用途 - Google Patents

1,4-雙(2-乙基己基)環己烷二甲酸酯在表面覆蓋物中作為增塑劑的用途 Download PDF

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Publication number
TW202246402A
TW202246402A TW111105267A TW111105267A TW202246402A TW 202246402 A TW202246402 A TW 202246402A TW 111105267 A TW111105267 A TW 111105267A TW 111105267 A TW111105267 A TW 111105267A TW 202246402 A TW202246402 A TW 202246402A
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Taiwan
Prior art keywords
pvc
filler
surface covering
plastisol
layer
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Application number
TW111105267A
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English (en)
Inventor
邁克爾 格瑞斯
伊姆克 舒爾茨
卡斯滕 格倫
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德商贏創運營有限公司
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Publication of TW202246402A publication Critical patent/TW202246402A/zh

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Abstract

本發明提供多層表面覆蓋物，其各自具有自含填充劑之PVC塑性溶膠獲得及自不含填充劑之PVC塑性溶膠獲得之層，其中之每一者包含增塑劑組成物，該增塑劑組成物包含1,4-雙(2-乙基己基)環己烷二甲酸酯。此類表面覆蓋物可用作地板覆蓋物或仿皮革。

Description

1,4-雙(2-乙基己基)環己烷二甲酸酯在表面覆蓋物中作為增塑劑的用途
本發明係關於多層表面覆蓋物，其各自具有至少一個自含填充劑之PVC塑性溶膠獲得及自不含填充劑之PVC塑性溶膠獲得之層，其中之每一者包含增塑劑組成物，該增塑劑組成物包含1,4-雙(2-乙基己基)環己烷二甲酸酯（bis(2-ethylhexyl) cyclohexane-1,4-dicarboxylate；下文亦稱為1,4-DEHCH）。此類表面覆蓋物可用作地板覆蓋物或仿皮革。
多層表面覆蓋物，尤其地板覆蓋物及仿皮革係已知的且以工業規模生產。此類表面覆蓋物由多層組成。至少一些層主要由聚氯乙烯（polyvinylchloride；PVC）組成，必須向其中添加增塑劑以改良特性，諸如延展性及可加工性。歐洲最著名之PVC的增塑劑係鄰苯二甲酸二異壬酯（diisononyl phthalate；DINP），其亦被認為係地板覆蓋物及仿皮革應用的標準。DINP提供可接受之膠凝特徵、中等黏度及尤其低揮發性。低揮發性尤其在所提及之應用中為至關重要的，以便減少生產期間或最終產物中的排放。在可撓性PVC製品之生產期間，由於高加工溫度，增塑劑將至少部分地蒸發且隨後在較冷位置處冷凝及/或滴落，且因此導致污染，其隨後需要不定時停止生產，且此可導致經濟損失。
眾所周知DINP為全球標準之一。市場需求亦導致甚至更大程度上使用不含鄰苯二甲酸酯之增塑劑（參見US 2016/0326346 A1）。最重要的不含鄰苯二甲酸酯之增塑劑中之一者為1,2-環己烷二甲酸二異壬酯（diisononyl cyclohexane-1,2-dicarboxylate；1,2-DINCH）。對苯二甲酸酯，例如對苯二甲酸二-2-乙基己酯（di-2-ethylhexyl terephthalate；DEHT或DOTP）同樣為鄰苯二甲酸酯或尤其DINP之可能的大容量替代物，但此等由於被視為鄰苯二甲酸酯家族之一部分，因此在公眾感知中反覆遇到接受問題。然而，此兩種增塑劑類別與DINP相比具有較低膠凝速度及較高揮發性。為了補償膠凝之弱點，有必要添加快速膠凝劑（gelator）。但快速膠凝劑通常具有相對高的揮發性且因此增加整體增塑劑組成物之製程揮發性。此外，快速膠凝劑之額外使用增加了調配成本，因為其通常相對昂貴。
本發明之目標為提供一種多層表面覆蓋物，其中所存在之PVC塑性溶膠層包括有利的增塑劑組成物。
藉由如技術方案1之本發明多層表面覆蓋物來達成目標。在附屬申請專利範圍中規定本發明之較佳組態。此類表面覆蓋物為多層表面覆蓋物，其包含至少一個自包含PVC、填充劑及增塑劑組成物之含填充劑之PVC塑性溶膠獲得的層及至少一個自包含PVC及增塑劑組成物之不含填充劑之PVC塑性溶膠獲得的層，其特徵在於該含填充劑之PVC塑性溶膠及該不含填充劑之PVC塑性溶膠中之該增塑劑組成物分別含有1,4-雙(2-乙基己基)環己烷二甲酸酯（1,4-DEHCH）。
當用於塑性溶膠中時，與其他環己烷二甲酸酯或此等酯之混合物相比，根據本發明之此增塑劑組成物使得總體效能得到改良。因此有可能甚至在不添加快速膠凝劑之情況下達成DINP的目標膠凝速度。此外，包含根據本發明之增塑劑組成物之塑性溶膠與包含DINP之塑性溶膠相比具有明顯的黏度降低，其導致塑性溶膠更快或更易於分散，及/或亦可有利地用於降低調配物成本，因為填充劑含量可增加。與其他環己烷二甲酸酯（例如1,4-DINCH、1,2-DINCH、1,2-DEHCH）相比，膠凝速度增加，其可引起較高加工速度或較低加工能量輸入。
在本發明之上下文中，措辭「自……獲得之層」意謂對應層係自對應塑性溶膠組成物獲得。為了生產根據本發明之表面覆蓋物，此處呈現之塑性溶膠以液體或自由流動形式使用，經由展開方法逐層施加，且接著在既不足以完全膠凝亦不足以發泡（100℃至150℃）之溫度下反覆地預膠凝化，其預先乾燥各層且能夠施加下一層，且在160℃至230℃之溫度下進行加工，僅在最終步驟得到最終產物，例如在所謂的「膠凝通道」。在此步驟中，接著亦發生個別層之發泡及「結合」。
根據本發明之表面覆蓋物的層原則上可以任何順序排列。但根據本發明較佳地，自含填充劑之PVC塑性溶膠獲得之層安置於自不含填充劑之PVC塑性溶膠獲得之層的下方。在自含填充劑之PVC塑性溶膠及自不含填充劑之PVC塑性溶膠獲得之兩個層之間，可存在一或多個其他層及/或載體材料，例如聚酯織物、玻璃非織物、紙或板。載體材料亦可較佳存在於含填充劑之層內的位置處。
含填充劑之PVC塑性溶膠除PVC以外亦含有填充劑及增塑劑組成物。不同類型之PVC可用作含填充劑之PVC塑性溶膠的PVC。含填充劑之PVC塑性溶膠中之PVC較佳為糊狀PVC、增補劑PVC或所提及之PVC類型中之兩種或更多種之混合物。在一替代性具體實例中，PVC為兩種或更多種糊狀PVC之混合物。
糊狀PVC與增補劑PVC之間的差異典型地為產生方式及所形成PVC粒子之所得粒度。可藉由乳液聚合或微懸浮聚合產生糊狀PVC，其提供通常具有1至40 µm之粒徑的PVC粒子。增補劑PVC可藉由懸浮聚合產生。所得之PVC之聚結粒子的粒徑通常為80至200 µm。添加增補劑PVC之一種效應為，甚至在增塑劑含量較低之情況下亦降低塑性溶膠之黏度水準，其使得塑性溶膠更容易擴展。
精確之組成根本上為可變的且可經調適用於對應應用。對於根據本發明之表面覆蓋物，較佳地，含填充劑之PVC塑性溶膠以每100質量份PVC之35至80質量份、較佳以每100質量份PVC之40至75質量份的比例含有增塑劑組成物。增塑劑組成物含有1,4-雙(2-乙基己基)環己烷二甲酸酯（1,4-DEHCH），但亦可含有一或多種其他增塑劑。相應增塑劑為所屬技術領域中具有知識者已知。在各情況下以總增塑劑組成物計，1,4-DEHCH尤其以至少50重量%、較佳至少65重量%且更佳至少80重量%之比例存在於增塑劑組成物中。在一尤其較佳之具體實例中，含填充劑之PVC塑性溶膠之增塑劑組成物僅由1,4-DEHCH組成。
根據本發明之用於多層表面覆蓋物之含填充劑之PVC塑性溶膠較佳以每100質量份PVC之50至200質量份、較佳以每100質量份PVC之70至180質量份、更佳以每100質量份PVC之85至170質量份的比例含有填充劑。適用於表面覆蓋物之填充劑為所屬技術領域中具有知識者已知。在本發明之上下文中可用於含填充劑之PVC塑性溶膠中之較佳填充劑為碳酸鈣、碳酸鎂、氧化鋁、矽酸鈣、滑石、硫酸鈣、氧化鈣、氧化鎂、矽酸鋁、白雲石、氧化矽及矽藻土。尤其較佳為碳酸鈣及碳酸鎂。
含填充劑之PVC塑性溶膠可另外含有添加劑以及所提及之成分。額外添加劑之實例為可以降低塑性溶膠之黏度的流變添加劑，且亦為環氧化植物油，諸如作為共穩定劑之環氧化大豆油（epoxidized soybean oil；ESBO），且亦為可降低表面張力之熱穩定劑或除氣劑，以便能夠更容易地自塑性溶膠中移除於塑性溶膠生產中形成之氣泡。流變添加劑之實例為以商標名VISCOBYK®-5120、VISCOBYK®-5130及VISCOBYK®-4041得到的產品。已知除氣劑為甲基烷基聚矽氧烷（可例如以商標名BYK®-3105獲得）或聚伸烷基衍生物（可例如以商標名BYK®-3155獲得）。較佳除氣劑不含聚矽氧。適合之熱穩定劑為鉛鹽、有機錫化合物、鋇/鋅化合物、鎘化合物或鋅化合物、鈣/鋅穩定劑及有機基穩定劑（organic-based stabilizer；「OBS」）。較佳熱穩定劑為鋇/鋅化合物、鈣/鋅穩定劑及有機基穩定劑（「OBS」）。添加劑可各自單獨地以每100質量份PVC之至多15質量份之量存在於塑性溶膠中。
多層表面覆蓋物亦可包含載體材料。多種材料可用作用於此處所描述之表面覆蓋物的載體材料。用於多層曲面覆蓋物之載體材料較佳地由聚酯織物、玻璃非織物、紙或板組成。若存在載體材料，則其至少在頂面上（亦即在一面上）塗佈有含填充劑之PVC塑性溶膠。此尤其係關於紙及紙板。作為塗佈之結果，自由流動之塑性溶膠組成物將滲透至載體材料之結構中。在本發明之上下文中，載體材料因此形成自含填充劑之PVC塑性溶膠獲得之層的一部分。載體材料較佳在兩面（亦即在頂面及底面）上塗佈有含填充劑之PVC塑性溶膠，其亦可在一個步驟中實現。此使得載體材料經含填充劑之PVC塑性溶膠浸漬。載體材料接著存在於自含填充劑之PVC塑性溶膠獲得之層中。
除PVC以外，不含填充劑之PVC塑性溶膠亦含有至少一種增塑劑組成物。根據其名稱，不含填充劑之PVC塑性溶膠不含有任何填充劑（亦即可視為填充劑之任何物質）。自不含填充劑之PVC塑性溶膠獲得之層較佳為透明的。不同類型之PVC可用作不含填充劑之PVC塑性溶膠的PVC。不含填充劑之PVC塑性溶膠中之PVC較佳為糊狀PVC、增補劑PVC或所提及之PVC類型中之兩種或更多種之混合物。在一替代性具體實例中，PVC為兩種或更多種糊狀PVC之混合物。已在上文中說明糊狀PVC與增補劑PVC之間的定義及差異。
對於不含填充劑之PVC塑性溶膠，較佳地其含有至少一種糊狀PVC及至少一種增補劑PVC。糊狀物PVC及增補劑PVC之量可在廣泛的範圍內變化且與各別應用之需求相匹配。在一較佳具體實例中，在各情況下以不含填充劑之PVC塑性溶膠中PVC之總量計，糊狀PVC以40重量%至80重量%之量存在且增補劑PVC以20重量%至60重量%之量存在。顯而易見，糊狀PVC及增補劑PVC之量必須合計為100重量%。
不含填充劑之PVC塑性溶膠之組成根本上為可變的且可經調適用於對應應用。對於根據本發明之表面覆蓋物，較佳地，不含填充劑之PVC塑性溶膠以每100質量份PVC之15至40質量份的比例含有包含1,4-DEHCH的增塑劑組成物。增塑劑組成物含有1,4-雙(2-乙基己基)環己烷二甲酸酯（1,4-DEHCH），但亦可含有一或多種其他增塑劑。相應增塑劑為所屬技術領域中具有知識者已知。在各情況下以總增塑劑組成物計，1,4-DEHCH尤其以至少50重量%、較佳至少65重量%且更佳至少80重量%之比例存在於增塑劑組成物中。根據本發明，較佳地，不含填充劑之PVC塑性溶膠以及1,4-DEHCH之增塑劑組成物包含快速膠凝劑。快速膠凝劑可以每100質量份PVC之至多15質量份的比例存在於不含填充劑之PVC塑性溶膠中。適合的快速膠凝劑為二苯甲酸乙二醇酯、對苯二甲酸二丁酯或對苯二甲酸二戊酯、苯甲酸2-乙基己酯、苯甲酸異壬酯或苯甲酸異癸酯、檸檬酸三丁酯、檸檬酸乙醯基三丁酯或具有C4至C7烷基鏈之氫化鄰苯二甲酸或對苯二甲酸酯。
不含填充劑之PVC塑性溶膠可另外含有添加劑以及所提及之成分。額外添加劑之實例為可降低塑性溶膠黏度之流變添加劑。已知流變添加劑之實例為以商標名VISCOBYK®-5120、VISCOBYK®-5130及VISCOBYK®-4041得到的產品。添加劑可以每100質量份PVC之3至12質量份、較佳4至10質量份的比例存在於不含填充劑之PVC塑性溶膠中。
另外，不含填充劑之PVC塑性溶膠可包含一或多種熱穩定劑。適合之熱穩定劑為鉛鹽、有機錫化合物、鋇/鋅化合物、鎘化合物或鋅化合物、鈣/鋅穩定劑及有機基穩定劑（「OBS」）。較佳熱穩定劑為鋇/鋅化合物、鈣/鋅穩定劑及有機基穩定劑（「OBS」）。不含填充劑之PVC塑性溶膠中之一或多種穩定劑的比例較佳為每100質量份PVC之1至4質量份。
根據本發明之多層表面覆蓋物可具有其他層以及已經提及之層。舉例而言，表面覆蓋物在反面上可具有自可發泡PVC塑性溶膠獲得之額外發泡層。此類層可改良聲學特性。在地板覆蓋物之情況下，自發泡PVC塑性溶膠獲得之此類層可用於減弱腳步聲。
自可發泡PVC塑性溶膠獲得之額外發泡層尤其包含PVC、包含至少1,4-雙(2-乙基己基)環己烷二甲酸酯（1,4-DEHCH）之增塑劑組成物、一或多種填充劑、發泡劑、助促進劑及視情況選用之一或多種額外添加劑。可發泡PVC塑性溶膠之額外發泡層之增塑劑組成物可另外包含快速膠凝劑。適合的快速膠凝劑為二苯甲酸乙二醇酯、對苯二甲酸二丁酯或對苯二甲酸二戊酯、苯甲酸2-乙基己酯、苯甲酸異壬酯或苯甲酸異癸酯、檸檬酸三丁酯、檸檬酸乙醯基三丁酯或具有C4至C7烷基鏈之氫化鄰苯二甲酸或對苯二甲酸酯。
自可發泡PVC塑性溶膠獲得之額外發泡層之組成根本上為可變的且可經調適用於對應應用。對於根據本發明之表面覆蓋物，較佳地，發泡PVC塑性溶膠之額外層以每100質量份PVC之40至80質量份的比例含有包含1,4-DEHCH的增塑劑組成物。發泡PVC塑性溶膠之額外層亦可以每100質量份PVC之70至200質量份的比例含有填充劑。
為實現所需發泡，可使用一或多種發泡劑。發泡劑分解而形成氣體（氣泡），其引起發泡。已知發泡劑之實例包括偶氮二甲醯胺、碳酸酯、碳酸氫鹽或氧代雙苯磺醯肼（oxybisbenzenesulfonylhydrazide；OBSH）。發泡劑典型地必須僅使用相對較小的量。然而，原則上，發泡劑之量與所需發泡程度相關。自可發泡PVC塑性溶膠獲得之額外發泡層以每100質量份PVC之2至5質量份的比例含有發泡劑。
根據本發明，發泡劑之分解可藉由所謂的助促進劑催化。所採用之助促進劑一般為含鋅化合物。適合之助促進劑為例如ZnO、ZnBO 3，且亦為Zn鹽，諸如辛酸鋅、NaZn或KZn或MgZn化合物。助促進劑典型地使用以較小的量，但類型及量亦對發泡劑之分解速度具有關鍵影響，且因此對在有限時間發泡過程期間形成之氣泡的量具有關鍵影響，該等氣泡會引起發泡。發泡PVC塑性溶膠之額外層亦可因此較佳以每100質量份PVC之1至5質量份的比例含有助促進劑。
自可發泡PVC塑性溶膠獲得之額外發泡層可另外含有添加劑以及所提及之成分。額外添加劑之實例為可降低塑性溶膠黏度之流變添加劑。流變添加劑之實例為以商標名VISCOBYK®-5120、VISCOBYK®-5130及VISCOBYK®-4041得到的產品。添加劑可以每100質量份PVC之4至10質量份的比例存在於可發泡PVC塑性溶膠中。
額外發泡層視情況有可能藉由機械發泡（亦即藉由在空氣中攪拌）進行製備，來代替發泡劑之前述化學分解。在此狀況下將所謂的泡沫穩定劑添加至相應塑性溶膠中，並非添加助促進劑及發泡劑，且此等防止所引入之空氣再次逃逸且使泡沫破裂。一般基於聚矽氧或肥皂之此類化合物為所屬技術領域中具有知識者已知，例如商標名為「BYK® 8070」或BYK® 8020。在一尤其較佳之具體實例中，此機械泡沫亦可用於浸漬載體材料。
在本發明之一較佳具體實例中，根據本發明之多層表面覆蓋物具有裝飾。在本發明之上下文中，裝飾意謂視覺及/或觸覺組態，例如藉由引入（印刷）油墨及/或壓印圖案。此類裝飾可施加至及/或壓印於自含填充劑之PVC獲得的層上。但亦有可能存在自PVC塑性溶膠獲得之額外（視情況發泡）裝飾層，在其上施加及/或壓印裝飾。自可發泡PVC塑性溶膠獲得之額外（視情況發泡）裝飾層尤其包含PVC、包含至少1,4-雙(2-乙基己基)環己烷二甲酸酯之增塑劑組成物、填充劑及視情況選用之發泡劑、助促進劑及/或一或多種添加劑。
在本發明之一尤其較佳之具體實例中，本發明之多層表面覆蓋物包含載體材料；至少一個自包含PVC、填充劑及增塑劑組成物之含填充劑之PVC塑性溶膠獲得的層；至少一個自包含PVC及增塑劑組成物之不含填充劑之PVC塑性溶膠獲得的層；及至少一個自包含PVC、增塑劑組成物、填充劑、發泡劑及助促進劑之可發泡PVC塑性溶膠獲得之發泡層。所使用之PVC塑性溶膠中之每一者的增塑劑組成物含有1,4-雙(2-乙基己基)環己烷二甲酸酯（1,4-DEHCH）。在一尤其較佳之具體實例中，多層表面覆蓋物包含另一耐刮擦層，該耐刮擦層較佳由聚胺甲酸酯或聚丙烯酸酯組成且為透明的。
最佳地，多層表面覆蓋物在不含填充劑之層與含填充劑之層之間含有另一含填充劑之層（尤其發泡層），向其中施加裝飾。可例如藉助於網印滾筒以一或多個步驟（單獨地針對所使用之各色彩）施加裝飾油墨。在此情況下，通常採用化學抑制之原理，其意謂亦可為彩色PVC塑性溶膠之印刷油墨可包括添加之抑制劑溶液，該溶液藉由在施加此層之位置處對助促進劑進行化學錯合以防止或減緩發泡劑之分解，從而使得在該位置處僅僅存在輕微發泡（若存在）。適合的抑制劑可商購，例如基於苯并三唑或硫脲。
對於根據本發明之表面覆蓋物，較佳為層之特定順序。此等層順序亦可見於說明性圖式圖1、圖2及圖3中。在基本具體實例中（參見圖1），多層表面覆蓋物包含至少一個自含填充劑之PVC塑性溶膠獲得的層（2）及至少一個自不含填充劑之PVC塑性溶膠獲得的較佳透明的層（1）。至少一個自不含填充劑之PVC塑性溶膠獲得之較佳透明層（1）在此處安置於至少一個自含填充劑之PVC塑性溶膠獲得之層（2）上方。 圖2展示較佳具體實例，其中除至少一個自不含填充劑之PVC塑性溶膠獲得的較佳透明層（1）及至少一個自含填充劑之PVC塑性溶膠獲得的層（2）以外，存在載體材料（3）及自可發泡PVC塑性溶膠獲得之發泡層（4）。在此具體實例中，載體材料（3）之兩面已塗佈有含填充劑之PVC塑性溶膠，且因此位於至少一個自含填充劑之PVC塑性溶膠獲得的層（2）內。在此層（2）下方，隨後安置自可發泡PVC塑性溶膠獲得的發泡層（4）。亦可設想載體材料僅在頂面上塗佈有含填充劑之PVC塑性溶膠。載體材料隨後將直接鄰接自可發泡PVC塑性溶膠獲得的發泡層（4）。 圖3展示另一較佳具體實例，其中額外存在視情況發泡之裝飾層（5）。接著將視覺（彩色）及/或觸覺（例如圖案之壓印）裝飾（6）施加於此層。此處，裝飾層（5）安置於至少一個自含填充劑之PVC塑性溶膠獲得的層（2）及至少一個自不含填充劑之PVC塑性溶膠獲得的較佳透明的層（1）之間。
在一尤其較佳之具體實例中，亦將耐刮擦層，較佳地聚胺甲酸酯或聚丙烯酸酯施加至自不含填充劑之PVC塑性溶膠獲得的較佳透明層，以便增加耐刮擦性或耐磨性。圖中未示出任何此類層。
根據本發明之多層表面覆蓋物可以所屬技術領域中具有知識者已知之方式藉由逐層施加仍自由流動之塑性溶膠而產生，視情況具有中間乾燥，例如藉助於加熱至約100至140℃之輥/膠凝滾筒，從而產生部分膠凝（亦即不完全膠凝），使得在不相互組合塑性溶膠之情況下進一步施加下一層為可能的。視情況選用之中間乾燥可例如用所謂的膠凝滾筒進行，亦即加熱至所需溫度之輥。
多層表面覆蓋物可用於各種應用。在本發明之一尤其較佳具體實例中，表面覆蓋物為地板覆蓋物或仿皮革，且用於對應應用。
本發明在下文中藉由實施例闡明。然而，此等實施例僅揭示說明性具體實例且不應視為限制性的。
實施例1-塑性溶膠生產
生產PVC塑性溶膠如例如用於製造地板覆蓋物之面塗層膜（不含填充劑之層）。塑性溶膠調配物中之量各自以質量份（parts by mass；phr）給出。調配物報告於表1中。 表1：塑性溶膠調配物
   phr
PVC（Vestolit P1430 K70 – Ultra；來自Vestolit公司） 100
增塑劑或增塑劑混合物 50
作為共穩定劑之環氧化大豆油 （Edenol D81；來自Emery Oleochemicals公司） 3
基於Ca/Zn之熱穩定劑 （Reagens SLX 781） 2
首先稱量出液體成分且隨後稱量出粉狀成分至PE燒杯中。用刮勺手動攪拌混合物，以此方式使得不再存在未濕潤之粉末。隨後使混合燒杯夾持在溶解器攪拌器之夾持裝置中。在接通攪拌器之後，速度緩慢增加至約2000轉/分鐘（revolutions per minute；rpm）。在彼時間期間，將塑性溶膠謹慎地除氣。出於此目的，將壓力調節至低於20毫巴之壓力。塑性溶膠一達到約30℃之溫度，則速度降低至約350 rpm。此後，使塑性溶膠在此速度下且在低於20毫巴的壓力下除氣9分鐘。此確保塑性溶膠之均勻化中不會存在過早部分膠凝。
塑性溶膠中使用以下增塑劑或以下增塑劑之混合物： 1,4-DEHCH = 1,4-雙(2-乙基己基)環己烷二甲酸酯（本發明，韓國Hanwha Chemical公司） 1,2-DEHCH = 1,2-雙(2-乙基己基)環己烷二甲酸酯（臺灣Nan Ya公司） DINP =鄰苯二甲酸二異壬酯（VESTINOL 9，來自Evonik Operations有限公司） 1,2-DINCH = 1,2-環己烷二甲酸二異壬酯（ELATUR CH，Evonik Operations有限公司） 1,4-DINCH = 1,4-環己烷二甲酸二異壬酯（藉由對苯二甲酸二異壬酯之環氫化來製備） DOTP =對苯二甲酸二辛酯（Eastman 168，來自美國Eastman公司） DPT =對苯二甲酸二戊酯（Elatur DPT，來自Evonik Operations有限公司） 2088 = Benzoflex 2088（二苯甲酸乙二醇酯之混合物，來自美國Eastman公司）
實施例2-測定塑性溶膠黏度
使用旋轉模式及CC27量測系統，用Physica MCR 101流變儀（安東帕德國有限公司（Anton Paar Germany GmbH））藉助於相關軟體來量測實施例1中產生之塑性溶膠之黏度。在塑性溶膠生產後已在25℃下平衡24小時之後進行量測。
量測涉及以下幾點： -    100 s -1之初步剪切持續60秒之時段，在此期間未獲取量測結果 -    自200 s -1至0.1 s -1之下降的剪切速率斜變。記錄30個量測點，各者之量測點持續時間為10秒。
量測在室溫下進行。在各情況下測定在100 s -1之剪切速率下獲得之黏度。
用在各情況下指定之增塑劑或增塑劑混合物在實施例1中生產之塑性溶膠的黏度量測結果列於表2中。
實施例3-膠凝特徵
在Physica MCR 101（來自安東帕）中用在剪應力控制下操作之平行板分析系統（PP25）以振盪模式檢查塑性溶膠之膠凝特徵。將額外溫度控制罩連接至系統以便達成最佳可能的熱分配。建立以下量測參數： 模式：溫度梯度（線性溫度斜變） 起始溫度：25℃ 終點溫度：180℃ 加熱/冷卻速率：5 K/min 振盪頻率：4-0.1 Hz斜變（對數） 循環頻率ω：10 s -1量測點之數目：63 量測點持續時間：0.5 min 自動間隙調整 恆定量測點持續時間 間隙寬度0.5 mm
分析程序： 使用刮勺將數滴待分析之不含氣泡的塑性溶膠施加至分析系統之下板。如此操作可確保在組裝分析系統之後，一些塑性溶膠有可能均勻地自分析系統流出（在任何方向上不超過約6 mm）。隨後將溫度控制罩安置在樣品上方且開始分析。此涉及測定所謂的塑性溶膠之複數黏度作為溫度的函數。膠凝過程之起始由複數黏度之急劇升高來識別。此黏度增加開始愈早，系統之膠凝能力愈佳。所獲得之量測曲線用於藉由內插法測定各塑性溶膠之溫度，在該等溫度下量測1000 Pa*s之複數黏度。結果列於表2中。
實施例4-膜生產
實施例1中產生之塑性溶膠各自經處理以得到厚度為1 mm之膜。
出於此目的，首先將高光澤度離型紙（來自意大利Sappi）修剪至30×44 cm之尺寸且插入Mathis烘爐之LTSV塗佈設備之夾持框架中。隨後將夾持框架置放於導引框架上，將Mathis烘爐（模型LTF）調整至200℃，且在達到該溫度後對該框架進行預加熱。隨後將塗佈棒插入夾持構件中，且經由初步實驗調整塗佈棒間隙以使得膠凝化結束時之膜厚度為1 mm（+/- 0.05 mm）。塑性溶膠藉助於塗佈棒在夾持離型紙上展開（速度3 m/min）。其後，移除塗佈棒且將夾持框架移動至烘爐中。在膠凝（在200℃下2分鐘）之後，將框架移出烘爐且在冷卻之後，自紙移除膜。
實施例5-經由玻璃轉化溫度實現之冷可撓性（DSC）
為量測，由根據實施例4之各別塑性溶膠產生之PVC膜上衝壓出小圓（Ø 4.5 mm）。在氮氣下用Mettler Toledo DSC 1使用以下設置在鋁坩堝（多孔坩堝蓋）中分析此樣品： 乾燥氮氣：                                              約45 ml（STP）/min（=標準ml/min） 氮氣（沖洗氣體）：                                 約180 ml（STP）/min 冷卻：                                                      液氮（輔助儲液罐1.5巴） 方法： [ 1]             25.0℃至120.0℃，25.0 K/min [ 2]             120.0℃，5.00 min等溫 [ 3]             120.0℃至-50.0℃，25.0 K/min [ 4]             -50.0℃至-120.0℃，10.0 K/min [ 5]             -120.0℃，3.00 min等溫 [ 6]             -120℃至50.0℃，10.0 K/min 同步接通
各種溫度斜變消除樣品之熱歷程，且因此有助於結果之較高再現性。對於玻璃轉化，評估來自斜變[6]之一階導數之峰最大值。所得熱流繪製為量測溫度的函數。
實施例6-膜中增塑劑之揮發性
將每個樣品用衝頭自實施例4中產生之PVC膜中衝壓出三個圓（圓；直徑：5 cm）。樣品在乾燥器中平衡16小時。
樣品圓在分析天平上稱量，且引入至金屬絲籃中，且後者藉由牛頭犬夾閉合。
將130 ml活性碳引入至錫罐（1 l，高型）中。接著將具有樣品之第一金屬絲籃置放在活性碳中間，且將另外130 ml活性碳施加至樣品圓。總而言之，錫罐因此逐層地填充有520 ml活性碳及3個裝有樣品的金屬絲籃。最後，再引入一個上層之130 ml活性碳。
將錫罐之多孔蓋無壓力地置放在罐上。將經填充之錫罐安置於加熱至120℃之加熱櫃中，以此方式使得櫃中之通風機不關閉且使罐彼此間不接觸。空氣交換及通風檔板各自設定為10%。在120℃下72小時後，將樣品再次自櫃取出且冷卻，接著將個別樣品自籃取出，在乾燥器中再調節16小時且隨後在分析天平上再稱重。所得質量差異由增塑劑損失產生。在各情況下，平均值由三種質量差異形成，且計算增塑劑之損失百分比。結果列於表2中。
實施例7-測定膜之肖氏A硬度
為測定肖氏硬度，將實施例1中產生之塑性溶膠傾入直徑為42 mm之圓形不鏽鋼澆鑄模具（重量：20 g）中。隨後在空氣循環乾燥箱中在200℃下之模具中膠凝25分鐘，冷卻且隨後移出，且在量測之前在氣候受控房間（25℃）中調節至少16小時。所獲得之試樣之厚度為約12 mm。
硬度量測根據DIN 53 505使用來自Zwick-Roell之肖氏A量測儀器進行；在各情況下量測結果在3秒之後讀出。在各試樣上三個不同位置處進行量測，且形成平均值。結果列於表2中。 表2：實施例2、3、5、6及7之量測結果
PM DINP 1,2-DINCH DOTP 1,4-DINCH 1,4-DEHCH
塑性溶膠黏度，以Pa*s為單位（實施例2） 5.3 3.1 6.3 2.9 2.8
在1000 Pa*s下之T，以℃為單位（實施例3） 80 90 85 87 80
T g，以℃為單位（實施例5） -41 -47 -39 -49 -43
在3天/120℃之後之膜的揮發性（實施例6） 2.7% 4.3% 3.9% 2.6% 5.5%
肖氏A硬度（實施例7） 81 84 83 82 77
                 
PM 1,2-DEHCH 1,2-DINCH + DPT (2:1) DOTP + DPT (3:1) DOTP/2088 5:1 1,4-DINCH + DPT (2:1)
塑性溶膠黏度，以Pa*s為單位（實施例2） 2.8 3.4 5.1 7 3.3
在1000 Pa*s下之T，以℃為單位（實施例3） 83 79 80 77 78
T g，以℃為單位（實施例5） -41    -41 -36 -33 -43
在3天/120℃之後之膜的揮發性（實施例6） 9.3% 10.1% 6.7% 4% 8.5%
肖氏A硬度（實施例7） 81 79 79 80 77
來自表2之結果可概述如下： ‒    本發明增塑劑1,4-DEHCH之黏度遠低於DINP之黏度。因此，有可能實現較高填充水準（較多填充劑）及/或省去使用降黏劑。此為有利的，因為有可能節約使用降黏劑之額外成本（例如物質成本、儲存物質之額外罐的成本），且另外有可能避免由於典型地具有較高揮發性之降黏劑的蒸發而導致的可能問題。可替代地，有可能利用高效率（表現為低得多的肖氏硬度）以節省增塑劑，且因此進一步減少排放。 ‒    根據實施例4用1,4-DEHCH作為增塑劑產生之膜的玻璃轉化溫度（T g）與使用DINP作為增塑劑之膜的玻璃轉化溫度相當。 ‒    本發明1,4-DEHCH即使在不添加快速膠凝劑之情況下，在根據實施例3之膠凝特徵方面亦具有與DINP相同的值。其他增塑劑1,2-DINCH、DOTP及1,4-DINCH可僅藉助於快速膠凝劑（此處：DPT）調節至類似膠凝特徵。但此亦引起揮發性之上升，亦即劣化（實施例6）。 ‒    1,4-DINCH確實顯示出所有混合物中最低的揮發性，且仍具有低黏度及最佳冷可撓性（實施例5），但諸如膠凝（實施例3）之其他特性明顯惡化。此處不可能僅依賴於一個參數；取而代之，有必要根據各種參數來考慮總體效能。 ‒    在所有DINP替代方案中本發明增塑劑1,4-DEHCH在關於膠凝、揮發性及效率（肖氏硬度、黏度、冷可撓性）之方面顯示出最佳總體效能。此外，不需要添加快速膠凝劑，其出於前述原因為有利的。
無
1:自不含填充劑之PVC塑性溶膠獲得的較佳透明層
2:自含填充劑之PVC塑性溶膠獲得的層

Claims (15)

  1. 一種多層表面覆蓋物，其包含至少一個自包含PVC、填充劑及增塑劑組成物之含填充劑之PVC塑性溶膠獲得的層及至少一個自包含PVC及增塑劑組成物之不含填充劑之PVC塑性溶膠獲得的層，其特徵在於該含填充劑之PVC塑性溶膠及該不含填充劑之PVC塑性溶膠中之該增塑劑組成物分別含有1,4-雙(2-乙基己基)環己烷二甲酸酯。
  2. 如請求項1之多層表面覆蓋物，其中該含填充劑之PVC塑性溶膠中及該不含填充劑之PVC塑性溶膠中之該PVC分別為乳液PVC、（微）懸浮PVC或此等之混合物。
  3. 如請求項2之多層表面覆蓋物，其中該不含填充劑之PVC塑性溶膠至少包含乳液PVC及（微）懸浮PVC。
  4. 如前述請求項中任一項之多層表面覆蓋物，其中該不含填充劑之PVC塑性溶膠以每100質量份PVC之15至40質量份的比例含有該增塑劑組成物。
  5. 如前述請求項中任一項之多層表面覆蓋物，其中該含填充劑之PVC塑性溶膠以每100質量份PVC之35至80質量份的比例含有該增塑劑組成物。
  6. 如前述請求項中任一項之多層表面覆蓋物，其中該含填充劑之PVC塑性溶膠以每100質量份PVC之50至200質量份的比例含有該填充劑。
  7. 如前述請求項中任一項之多層表面覆蓋物，其中該多層表面覆蓋物包含至少一種載體材料，該載體材料之一面或兩面已塗佈有含填充劑之PVC塑性溶膠。
  8. 如請求項7之多層表面覆蓋物，其中該載體材料由聚酯織物、玻璃非織物、紙或板組成。
  9. 如前述請求項中任一項之多層表面覆蓋物，其中該表面覆蓋物在其反面上具有自可發泡PVC塑性溶膠獲得之額外發泡層。
  10. 如請求項9之多層表面覆蓋物，其中該可發泡PVC塑性溶膠包含PVC、增塑劑組成物、填充劑、發泡劑及助促進劑（kicker），以及視情況選用之用於降低黏度的添加劑。
  11. 如請求項9或10之多層表面覆蓋物，其中自可發泡PVC塑性溶膠獲得之該額外發泡層以每100質量份PVC之70至200質量份的比例含有該填充劑。
  12. 如請求項9或11中任一項之多層表面覆蓋物，其中自可發泡PVC塑性溶膠獲得之該額外發泡層以每100質量份PVC之40至80質量份的比例含有該增塑劑。
  13. 如請求項9或12中任一項之多層表面覆蓋物，其中該多層表面覆蓋物包含載體材料；至少一個自包含PVC、填充劑及增塑劑組成物之含填充劑之PVC塑性溶膠獲得的層；至少一個自包含PVC及增塑劑組成物之不含填充劑之PVC塑性溶膠獲得的層；及至少一個自包含PVC、增塑劑組成物、填充劑、發泡劑及助促進劑之可發泡PVC塑性溶膠獲得之發泡層，其特徵在於所使用之該等PVC塑性溶膠中之每一者的該增塑劑組成物含有1,4-雙(2-乙基己基)環己烷二甲酸酯。
  14. 如請求項13之多層表面覆蓋物，其中該多層表面覆蓋物另外亦包含耐刮擦層，該耐刮擦層較佳由聚胺甲酸酯或聚丙烯酸酯組成且為透明的。
  15. 一種如前述請求項中任一項之多層表面覆蓋物之用途，其用作地板覆蓋物或仿皮革。
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US20220259451A1 (en) 2022-08-18
JP2022125019A (ja) 2022-08-26
KR20220117162A (ko) 2022-08-23
EP4043517A1 (de) 2022-08-17
CA3148512A1 (en) 2022-08-16

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