TW201910387A - 氣凝膠／複合非織物防火隔熱材之製備方法 - Google Patents

氣凝膠／複合非織物防火隔熱材之製備方法 Download PDF

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TW201910387A
TW201910387A TW106127828A TW106127828A TW201910387A TW 201910387 A TW201910387 A TW 201910387A TW 106127828 A TW106127828 A TW 106127828A TW 106127828 A TW106127828 A TW 106127828A TW 201910387 A TW201910387 A TW 201910387A
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aerogel
solution
coupling agent
silane coupling
woven
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TW106127828A
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TWI643888B (zh
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陳建宏
陳秀秀
張智舜
李勁直
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崑山科技大學
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Priority to TW106127828A priority Critical patent/TWI643888B/zh
Priority to CN201711182197.5A priority patent/CN109403022B/zh
Priority to US15/873,712 priority patent/US10669392B2/en
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Abstract

本發明關於一種氣凝膠/複合非織物防火隔熱材之製備方法，包括下列步驟：提供一烷氧化矽類與一矽膠類進行混合，再添加一矽烷偶合劑類繼續攪拌，隨後滴入酸觸媒進行水解反應，過程中再添加矽烷偶合劑水溶液繼續攪拌；隨後再加入含水鹼觸媒(以及不含水鹼觸媒)有機水溶液進行縮合反應，以形成矽膠-矽氣凝膠-矽偶合劑溶液；將前述溶液含浸加入複合非織物毯，並經熟成以及自然乾燥程序，以形成一具柔軟之疏水性(以及親水性)氣凝膠/複合非織物防火隔熱材，可同時大量生產不同親疏水表面性質且柔軟性之氣凝膠/複合非織物材料，作為產業高溫設備的隔熱材料或建築結構的室內隔熱與防火板材之用途。

Description

氣凝膠/複合非織物防火隔熱材之製備 方法
本發明係有關於一種不同表面親疏水性質且柔軟性之氣凝膠/複合非織物防火材之製備方法，尤指結合矽酸甲酯(TMOS)或矽酸乙酯(TEOS)或R-稀烃基矽酸甲酯(RTMS)或R-基矽酸乙酯(RTES)或R-稀烃基矽膠或R-稀烃基矽偶合劑混合物的矽氣凝膠-矽膠-矽偶合劑三混合氣凝膠溶液體系；隨後將此三混合氣凝膠溶液含浸加入一複合非織物毯，使前述氣凝膠混合溶液均勻穿插在該非織物中，並經一熟成以及自然乾燥程序，以形成一不同親疏水表面性質且柔軟性之氣凝膠/複合非織物材料，應用於高溫設備的隔熱材料或建築結構的室內隔熱以及防火板材之用途。
按，氣凝膠擁有許多的特殊性質，如低密度、高孔隙率、高比表面積以及低熱傳導係數。目前針對氣凝膠的製備方法係以溶膠凝膠合成法，由烷氧化矽類(Alkoxysilane)或正矽酸甲酯等前驅物與含水有機溶 劑進行混合後，添加酸觸媒，進行水解反應(Hydrolysis)。水解一定時間後，再添加鹼觸媒，進行縮合反應(Condensation)，反應後會形成溶膠。溶膠內的分子繼續進行縮合反應鍵結，逐漸形成半固態的高分子凝膠，再經過一段時間的熟化，膠體會形成結構穩定的3D立體網狀結構。
而氣凝膠可利用化學劑進行改質，其機制為將氣凝膠表面的氫氧(-OH)官能基與改質劑上的氯(-Cl)反應產生鹽酸，然後取代氫(-H)，改質為疏水的-OSi(CH3)3官能基。此種疏水的官能基，在氣凝膠常壓乾燥的過程中，可以減少表面張力的大小，在極小量的體積收縮下，仍能保有溼凝膠的3D立體網狀結構。
傳統氣凝膠材料，因含有大量的水分子，故其乾燥製程需利用二氧化碳超臨界乾燥機進行乾燥，而製程條件係在溫度攝氏34度下以高壓將液態二氧化碳轉變成超臨界條件，並利用超臨界二氧化碳將氣凝膠中水分子溶出乾燥。惟，此製程並無法工業化製程，相對所製備的氣凝膠也會明顯形成龜裂而破碎，進而影響氣凝膠的整體工業應用，故製備上仍有相當改善的空間。
目前國內外一些有關氣凝膠材料專利的先前技術資料，略舉如下：
1.美國專利第8,029,871號「生產二氧化矽氣凝膠塗層的方法」，揭示二氧化矽氣凝膠塗料係由烷氧基矽烷和有機改性劑進行水解以及聚合所獲得濕的有機改性二氧化矽凝膠，利用超聲波處理所製備的形成有機改性二氧化矽凝膠形成有機改性的二氧化矽分散物，添加紫外線固化型樹脂和光聚合引發劑於此有機改性的二氧化矽分散物形成二氧化矽氣凝膠塗料液體，應用此塗料液體於基材上，然後照射紫外線於此塗層。
2.美國專利第8,021,583號「含有氣凝膠毯子」，係形成毯子的製程描述，意謂形成型疏水性氣凝膠漿液，纖維和至少一個潤濕劑，乾燥此漿液形成一極大的乾燥產品，並將該乾燥產品製成毛毯，以應用在各層面。
3.另有相關前案如中華民國發明專利編號第103135659號之「氣凝膠/非織物複合防火/隔熱材及其製備方法」，主要係說明將一烷氧化矽類或一正矽酸甲酯在一低含水有機溶液中進行混合，並添加一酸觸媒，以進行一水解反應。再添加一鹼觸媒無水有機溶液以進行縮合 反應，形成凝膠化之一氣凝膠。將前述氣凝膠加入一非織物中，使前述氣凝膠充分穿插在該非織物中，並經一乾燥程序，以形成一氣凝膠/非織物複合隔熱材。藉此，能大量產製出本發明之氣凝膠/非織物複合隔熱材，作為隔熱材或防火材之用途。
爰此，本發明人有鑑於先前氣凝膠應用於隔熱或多孔吸附應用專利眾多，但尚無利用矽膠以及矽氣凝膠二混合氣凝膠溶液含浸於複合非織物中形成介面接著完整且相互穿插網狀結構的氣凝膠/複合非織物材料，尤指可同時大量生產不同表面親疏水性質且柔軟性之氣凝膠/複合非織物材料，作為產業高溫設備的隔熱材料或建築結構的室內隔熱以及防火板材之用途的專利。因此本專利提出一種結合複合非織物以及複合氣凝膠溶液以製備出氣凝膠/非織物複合隔熱、防火材料及其製備方法。藉由結合矽膠-矽氣凝膠以及複合非織物的複合材料兼具柔軟性、高防火、高隔熱等特性目的。
本發明提供一種混合氣凝膠溶液以及複合非織物以製備兼具柔軟以及防火性質的氣凝膠/複合非織物材料製備方法，混合氣凝膠溶液包括有下列步驟： (S1)混合步驟：提供將一矽酸甲酯(Tetramethoxysilane,TMOS)或矽酸乙酯(Tetraethoxysilane,TEOS)或R-稀烃基矽酸甲酯(RTMS)或R-基矽酸乙酯(RTES)或R-稀烃基矽膠混合物混合後加一有機混合溶液在高速攪拌下混合均勻，其中烷氧化矽類與矽膠類的莫耳比(mol：mol)為1.0：0.001至1.0：5.0。
隨後再添加一微量的R-稀烃基矽偶合劑於此溶液中在繼續攪拌反應，使R-稀烃基矽偶合劑再結合於氣凝膠結構上，其中添加R-稀烃基矽膠以及矽烷偶合劑於矽膠-氣凝膠結構中為降低氣凝膠的親水性質以增加矽膠-矽氣凝膠-R-稀烃基矽偶合劑結構中的R-官能基與非織物纖維中(PP、PET、玻纖或岩棉等)之間的化學結合，並增加矽膠-氣凝膠分子在含水有機溶液中的聚集能力以及增加氣凝膠的穩定性。其中，該烷氧化矽類：矽膠類：矽烷偶合劑類的莫耳比為1.0：0.01：0.001至1.0：0.65：1.0。該水解溶液中矽膠-矽氣凝膠-矽烷偶合劑混合物與含水有機溶液的體積比為5：95至100：200。該水解溶液中含水有機溶液中水的莫耳含量(mol%)由0mol%至80mol%。
(S2)水解步驟：隨後滴入含水酸觸媒(係硫酸H2SO4、磷酸H3PO4、硝酸HNO3、鹽酸HCl等混合酸或單一酸當任酸觸媒)於混合溶液中進行一水解反應；水解反應後，將會獲得一透明之矽膠-矽氣凝膠-矽烷偶合劑三混合氣凝膠溶液。其中所添加酸的含量越高，水解速率越快。
(S3)縮合步驟：提供一鹼觸媒之含水有機溶液所配置成之一鹼觸媒含水有機溶液，並逐漸加入至該氣凝膠混合溶液中，進行一縮合反應，以形成凝膠化之親水矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液體系。
(S30)另一縮合步驟：提供一鹼觸媒之不含水有機溶液所配置成之一鹼觸媒不含水有機溶液，並逐漸加入至該氣凝膠混合溶液中，以進行縮合反應，以形成凝膠化之疏水性質矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液體系。該縮合溶液中含水有機溶液中水的莫耳含量(mol%)由0mol%至80mol%。其中，該鹼觸媒有機溶液中鹼觸媒(NaOH、NaHCO3、Na2CO3、NH4OH混合鹼溶液或單一鹼溶液)與(2)氣凝膠溶液的酸觸媒的莫耳比為1.02比1至3比1，鹼莫耳比越大，則氣凝膠溶液的凝膠化速率越快。
(S4)氣凝膠/複合非織物材料的成型步驟：取前述含水凝膠化的矽膠-矽氣凝膠-矽烷偶合劑氣凝膠含水混合溶液含浸一回收復合非織物毯或一般復合非織物毯，使前述矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液充分與非織物完全結合反應，並隨後矽膠-矽氣凝膠-矽烷偶合劑凝膠溶液凝膠化，在此過程中以製備出一表面親水性氣凝膠結合複合非織物材料。
(S40)另一成型步驟：取前述不含水凝膠化的矽膠-矽氣凝膠-矽烷偶合劑氣凝膠含水混合溶液含浸一回收復合非織物毯或一般復合非織物毯，使前述矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液充分與非織物完全結合反應，並隨後矽膠-矽氣凝膠-矽烷偶合劑凝膠溶液凝膠化，在此過程中以製備出一表面疏水性氣凝膠結合複合非織物材料矽膠-矽氣凝膠-矽烷偶合劑氣凝膠穿插在該非織物中。
(S5、S50)隨後經一常壓自然乾燥步驟，以形成具柔軟及多孔性一親水性氣凝膠/非織物複合材(S5)；以及形成具柔軟及多孔性一疏水性氣凝膠/複合非織物材(S50)。隨後再將溫度升溫80℃溫度條件下使氣凝膠/複合非織物材進行快速脫乙醇，並隨後再將溫度升溫 至105-120℃溫度條件下使氣凝膠/非織物複合材進行快速脫水乾燥，藉此，獲得一具柔軟及多孔性之氣凝膠/複合非織物材料。
其中，本發明之使用矽膠(Poly(dimethenesilicone，PDMS、MDMS)為雙末端雙官能基或雙末端加測鏈之叁至肆官能基之矽膠結構，本實驗所使用的矽膠(PDMS或MDMS)官能基可為酸基(-COOH)、胺基(-NH2)、羥基(-OH)、縮酸基、環氧基、醚基等。
進一步，該酸觸媒係H2SO4+H3PO4、HNO3+HCl混合酸或單一酸當任酸觸媒，而該第一含水有機溶液係選自：水、C1-C5醇類、C1-C5酸類、C1-C5酯類或C1-C5醚類所構成群組之一或其組合，其中，該烷氧化矽類：矽膠類：矽烷偶合劑類的莫耳比為100：2.5：0.1至100：65：10。其中矽膠-矽氣凝膠-矽烷偶合劑氣凝膠固體含量在整體氣凝膠含水有機溶液中體積百分比(V/V%)介於5.0%至95.0%。其中含水有機溶液的含量越高，乾燥後氣凝膠體機內部孔洞含量越高，當含水有機溶液的含量高於50.0%以上時，含水有機溶劑之間的孔洞將會逐漸連結而形成連續式孔洞。
進一步，在(S2)溶液中該酸觸媒的莫耳百分比(mol%)為百分之0.001至百分之0.1，其中，酸觸媒的莫耳百分比增加可增加烷氧化矽類、矽膠類以及矽烷偶合劑之間進行化學鍵結合而形成共聚合反應。
進一步，在(S3)溶液中該鹼觸媒係NaOH、NaHCO3、Na2CO3、NH4OH混合鹼溶液或單一鹼溶液，而該第二含水有機溶液係選自：水、C1-C5醇類、C1-C5氨類、C1-C5酯類或C1-C5醚類所構成群組之一或其組合。
進一步，該觸媒有機溶液中鹼觸媒與(S2)氣凝膠溶液的酸觸媒的莫耳比為1.02：1至3.0：1，其中鹼觸媒莫耳比越大，則氣凝膠溶液的縮合反應越快，使矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液的縮合反應時間由1100分鐘縮短至3-5分鐘。
進一步，前述(S4；S40)成型步驟中取尚未凝膠化的矽膠-矽氣凝膠-矽烷偶合劑氣凝膠混合溶液含浸一回收複合非織物毯或一般複合非織物毯，使前述矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液充分與非織物完全含浸，並隨後矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液凝膠化，在此過程中矽膠-矽氣凝膠-矽烷偶合劑氣凝膠穿插在 該非織物中，並隨後經一自然乾燥程序，以形成一具柔軟及多孔性之氣凝膠/非織物複合材。
進一步，前述(S4；S40)成型步驟中所述將前述矽膠-矽氣凝膠-矽烷偶合劑氣凝膠混合溶液充分與非織物形成相互穿插結構，在該成型步驟中係透過噴塗、淋噴、含浸加工或溶液連續壓吸加工等方式進行實現。
該乾燥程序之條件為常壓下攝氏30度至80度，溫度越高乾燥時間下降，乾燥時間由3600分鐘降低至150分鐘。
進一步，該氣凝膠/非織物複合隔熱材中所含該三混合矽膠-矽氣凝膠-矽烷偶合劑氣凝膠與非織物纖維的體積百分比(V/V%)含量為百分之25至百分之70。
進一步，該複合非織物毯係由聚丙烯(PP)、聚對苯二甲酸乙二醇酯(PET)或聚醯胺(Nylon)、玻纖、岩棉、碳纖棉其中之一或其組合所製成。
本發明再提供一種氣凝膠/非織物複合材，係使用前述矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液以及複合非織物利用連續式噴灑加工、連續式噴霧加工、連續式壓吸加工、含浸加工等加工方式均可製備氣凝膠/複合非織物材料。其中，該氣凝膠/非織物複合材包含有一 複合非織物及一混合矽膠-矽氣凝膠-矽烷偶合劑氣凝膠，該混合氣凝膠與該非織物結合形成相互穿插的立體網狀結構。
進一步，該矽烷偶合劑為一含稀烃類或含長鏈稀烃類矽烷結構，另其反應機團可為氯化矽烷偶合劑、稀基矽烷偶合劑、環氧基矽烷偶合劑、酸基矽烷偶合劑、胺基矽烷偶合劑、羥基矽烷偶合劑或縮酸基矽烷偶合劑等。
本發明之功效在於：
1.藉由結合具柔軟且多孔性之矽膠-矽氣凝膠-矽烷偶合劑氣凝膠材料的高防火、隔熱特性以及氣凝膠/複合非織物材料表面親疏水性質可調性，並結合非織物的柔軟及力學性質以形成不同親疏水表面性質的氣凝膠/複合非織物材料，並能在常溫常壓條件下進行大量製造，以應用防火、隔熱建材、高溫工廠設施等各式防火、隔熱材料以及汽車或一般民生用隔音、隔熱材料等應用。
2.本發明中藉由調整該矽膠-矽氣凝膠-矽烷偶合劑氣凝膠中各成分含量以調整該矽膠-矽氣凝膠-矽烷偶合劑氣凝膠的親疏水性質以及氣凝膠及複合非織 物間的結合能力，以改善目前氣凝膠與非織物之間結合能力弱所導致掉粉屑等問題。
3.本發明中藉由調整該酸觸媒的濃度以控制矽膠-矽氣凝膠-矽烷偶合劑的水解共反應時間。當該酸觸媒濃度為莫耳百分比0.001M時水解時間需達4小時，當該酸觸媒濃度為莫耳百分比0.1M時水解時間縮短至20分鐘。
4.本發明中藉由調整該鹼觸媒有機溶液中鹼觸媒含量以調整該縮合反應形成凝膠的時間。當該鹼觸媒的莫耳比含量對酸觸媒為1.02：1時凝膠化時間約16小時；而鹼觸媒的莫耳比含量對酸觸媒為3.0：1時凝膠化時間縮短至約3-5分鐘，藉以控制矽膠-矽氣凝膠-矽烷偶合劑凝膠溶液的微相分離行為及氣凝膠微結構，並可控制氣凝膠/非織物複合料的製程加工時間。
5.本發明係於水解反應後形成矽膠-矽氣凝膠-矽烷偶合劑混合氣凝膠溶液，利用矽膠-矽氣凝膠-矽烷偶合劑化學結合過程中矽膠、矽烷偶合劑分子中化學結構官能基的親、疏水基團比例，以破壞水分子內縮力所導致的破裂以及收縮現象。因此使矽膠-矽氣凝膠-矽烷偶合劑氣凝膠可進行一般常溫常壓條件下的進行乾燥，且在 該乾燥程序中矽膠-矽氣凝膠-矽烷偶合劑分子氣凝膠的收縮率將會明顯下降。藉以改善傳統氣凝膠體系中含水分子汽化過程中，因水的表面張力導致氣凝膠收縮或龜裂瓦解的現象，以改善純氣凝膠的易脆性質，增加該非織物在隔熱或阻熱上的機能。
6.在本發明該縮合步驟：利用提供一含水或不含水鹼觸媒之有機溶液所配置成之一含水或不含水鹼觸媒有機溶液，進行一縮合反應，可同時製備不同親水性以及疏水性的矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液體系。
7.本發明中該成型步驟中將不同親水性以及疏水性的矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液體系含浸一複合非織物毯，使前述矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液充分與非織物完全結合，可製備表面不同親疏水特性之多孔性之氣凝膠/非織物複合材。
8.本發明中該複合非織物係利用聚乙烯(PE)、聚丙烯(PP)、聚乙丙烯(PPE)、聚酯(Polyester)、聚醯胺(Polyamine)、玻璃纖維(glass fiber)以及岩棉其中之一或其組合之塑料所製備而成。並於矽膠-矽氣凝膠-矽烷偶合劑分子氣凝膠溶液凝膠化 後，使矽膠-矽氣凝膠-矽烷偶合劑氣凝膠與該非織物結合形成相互穿插的三次元網狀結構，達到結合力強，不易脫落之效果。
9.本發明中該未改質之親水性氣凝膠/複合非織物材料可在常壓常溫中進行乾燥。隨後再將溫度升溫至105-120℃溫度條件下矽膠-矽氣凝膠-矽烷偶合劑氣凝膠分子間進行快速脫水。
S1‧‧‧混合步驟
S2‧‧‧水解步驟
S3‧‧‧縮合步驟
S30‧‧‧另一梭合步驟
S4‧‧‧成型步驟
S40‧‧‧另一成型步驟
S5‧‧‧乾燥步驟
S50‧‧‧另一乾燥步驟
[第一圖]係為本發明之氣凝膠/複合非織物防火隔熱材之製備方法流程圖；[第二圖]係為本發明中不同配方所製備不同柔軟性氣凝膠/複合非織物防火隔熱材照片；[第三圖]係為本發明中利用矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液體系中含水量可調控所製備複合材料表面親疏水性質照片；及[第四圖]係為本發明中氣凝膠/複合非織物防火隔熱材表面及斷面之掃描式電子顯微鏡(SEM)照片。
為了讓本發明之氣凝膠/複合非織物防火隔熱材之製備方法的目的、特徵、和優點能更明顯易懂，下文特舉較佳實施例，並配合所附圖示，作詳細說明如下： 首先，請參閱第一圖所示，係本發明之氣凝膠/複合非織物防火隔熱材之製備方法流程圖。本發明提供一種可同時製備親水性及疏水性氣凝膠/複合非織物防火材料製備方法，其中製備親水性及疏水性氣凝膠/複合非織物防火材料包括有下列步驟：(1)混合步驟(S1)：提供一烷氧化矽類，在本發明實施例中係以四乙基矽氧烷(Tetraethoxysilane,TEOS)為範例說明，與一矽膠類，在本發明實施例中係以聚二甲基矽膠(Poly(dimethenesilicone,PDMS)。將一矽酸甲酯(TMOS)或矽酸乙酯(TEOS)或R-稀烃基矽酸甲酯(RTMS)或R-基矽酸乙酯(RTES)或R-稀烃基矽膠混合物混合後加一有機混合溶液在高速攪拌下混合均勻，其中烷氧化矽類與矽膠類的莫耳比(mol：mol)為100：0.5。
隨後再添加一微量的R-稀烃基矽偶合劑於此溶液中在繼續攪拌反應，使R-稀烃基矽偶合劑再結合於氣凝膠結構上，其中添加R-稀烃基矽膠以及矽烷偶合劑於矽膠-氣凝膠結構中為降低氣凝膠的親水性質以增加矽膠 -矽氣凝膠-R-稀烃基矽偶合劑結構中的R-官能基與非織物纖維中(PP、PET、玻纖或岩棉等)之間的化學結合，並增加矽膠-氣凝膠分子在含水有機溶劑中的聚集能力以及增加氣凝膠的穩定性及柔軟性質。請參閱第二圖所示，顯示本發明中不同配方所製備不同柔軟性氣凝膠/複合非織物防火隔熱材照片。
其中，該烷氧化矽類：矽膠類：矽烷偶合劑類的莫耳比(mol：mol：mol)為100：0.5：0.1。該水解溶液中矽膠-矽氣凝膠-矽烷偶合劑混合物與含水有機溶液的體積比為5：95。該水解溶液中含水有機溶液中水的莫耳含量(mol%)由50mol%。
(2)水解步驟(S2)：隨後滴入含水酸觸媒(H2SO4溶液)0.001mol%於混合溶液中進行一水解反應；水解反應後，將會獲得一透明之矽膠-矽氣凝膠-矽烷偶合劑三混合氣凝膠溶液。
(3)縮合步驟(S3)：提供一鹼觸媒(NaOH溶液)0.0015mol%以及含水有機溶液所配置成之一鹼觸媒含水有機溶液，並逐漸加入至矽膠-矽氣凝膠-矽烷偶合劑混合溶液中，進行一縮合反應，以形成凝膠化之親水矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液，其中，該鹼觸媒 含水有機溶液中鹼觸媒(NaOH溶液)與(2)氣凝膠溶液的酸觸媒(H2SO4)的酸鹼莫耳比為1.5比1，利用添加鹼觸媒催化矽膠-矽氣凝膠-矽烷偶合劑進行縮合反應，並促使矽膠-矽氣凝膠-矽烷偶合劑分子兼具及形成局部三次元結構。
(S30)另一縮合步驟：提供一鹼觸媒之不含水有機溶液所配置成之一鹼觸媒不含水有機溶液，並逐漸加入至該氣凝膠混合溶液中，以進行縮合反應，以形成凝膠化之疏水性質矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液體系。該縮合溶液中含水有機溶液中水的莫耳含量(mol%)由0mol%至80mol%。其中，該鹼觸媒有機溶液中鹼觸媒(NaOH、NaHCO3、Na2CO3、NH4OH混合鹼溶液或單一鹼溶液)與(2)氣凝膠溶液的酸觸媒的莫耳比為1.02比1至3比1，其中鹼莫耳比越大，則氣凝膠溶液的凝膠化速率越快。
(4)氣凝膠/複合非織物材料的成型步驟(S4)：取前述尚未凝膠化的矽膠-矽氣凝膠-矽烷偶合劑氣凝膠混合溶液含浸一複合非織物毯(70%E-glass玻纖棉混合30%PP纖維)，使前述矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液充分與複合非織物完全含浸，並隨後使溶液凝 膠化及熟化，在此過程中矽膠-矽氣凝膠-矽烷偶合劑氣凝膠穿插在該複合非織物中，在此過程中以製備出一表面親水性氣凝膠結合複合非織物材料。
(S40)另一成型步驟：取前述不含水凝膠化的矽膠-矽氣凝膠-矽烷偶合劑氣凝膠含水混合溶液含浸一回收復合非織物毯或一般復合非織物毯，使前述矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液充分與非織物完全結合反應，並隨後矽膠-矽氣凝膠-矽烷偶合劑凝膠溶液凝膠化，在此過程中以製備出一表面疏水性氣凝膠結合複合非織物材料矽膠-矽氣凝膠-矽烷偶合劑氣凝膠穿插在該非織物中。
(5)並隨後經一常溫常壓下自然乾燥步驟(S5)：使濕式氣凝膠/複合非織物材料進行氣凝膠乾燥，或利用攝氏30度至80度間進行有機溶液快速汽化乾燥程序、使前述氣凝膠中所含水有機溶液氣化蒸發，隨後再將溫度升溫至105-120℃溫度條件下使氣凝膠/非織物複合材進行快速脫水乾燥，令乾燥後的前述氣凝膠與該非織物呈現相互穿插的立體網狀結構，以形成一多孔性性氣凝膠/複合非織物材料，藉此，獲得一具柔軟及多孔性一親水 性氣凝膠/非織物複合材(S5)；以及形成具柔軟及多孔性一疏水性氣凝膠/複合非織物材(S50)。
該矽烷偶合劑為一含稀烃類或含長鏈稀烃類矽烷結構，另其反應機團可為氯化矽烷偶合劑、稀基矽烷偶合劑、環氧基矽烷偶合劑、酸基矽烷偶合劑、胺基矽烷偶合劑、羥基矽烷偶合劑或縮酸基矽烷偶合劑等。
較佳的是，該酸觸媒係硫酸H2SO4、磷酸H3PO4、硝酸HNO3、鹽酸HCl等混合酸或單一酸當任酸觸媒，而該第一含水有機溶液係選自：水、C1-C5醇類、C1-C5酸類、C1-C5酯類或C1-C5醚類所構成群組之一或其組合，其中，該烷氧化矽類：矽膠類：矽烷偶合劑類的莫耳比為100：2.5：0.1至100：65：10。其中矽膠-矽氣凝膠-矽烷偶合劑氣凝膠固體含量在整體氣凝膠含水有機溶液中體積百分比(V/V%)介於3.0%至45.0%。
如第三圖(a)及(b)所顯示，氣凝膠整體溶液體系中含水有機溶液的含量對氣凝膠/複合非織物表面親疏水性質影響照片。製備氣凝膠整體溶液體系中含水有機溶液的含量高於10.0%以上時，含水有機溶劑之間親水基團作用力將會將矽膠-矽氣凝膠-矽烷偶合劑氣凝膠體系中疏水基團(如矽膠分子鏈及矽烷偶合劑疏水基團) 排除在整體氣凝膠結構外圍，因此導致形成一表面疏水性質的矽膠-矽氣凝膠-矽烷偶合劑氣凝膠結合複合非織物纖維複合材料(第三圖(a))。
製備氣凝膠整體溶液體系中含水有機溶液的含量小於10.0%以上時，可製備表面親水性質的氣凝膠/複合非織物纖維複合材料(第三圖(b))，另外將氣凝膠體系中所形成的奈米孔洞將會逐漸連結而形成連續式的介孔或微孔孔洞。在本發明較佳實施例中，該烷氧化矽：矽膠：矽烷偶合劑的莫耳比為100：0.5：0.01。該水解溶液中矽膠-矽氣凝膠-矽烷偶合劑混合物與含水有機溶液的體積比為10：90。該水解溶液中含水有機溶液的水的莫耳含量(mol%)為50mol%。
在本發明中，該氣凝膠之製備係以習知溶膠凝膠合成法為基礎做改良後所製得，在本發明專利中利用在酸性條件下使矽膠分子、矽氣凝膠分子以及矽烷偶合劑相互之間進行化學鍵結，以改善前述習知方法之缺點。第四圖(a)及(b)分別為矽膠-矽氣凝膠-矽烷偶合劑氣凝膠/複合非織物防火隔熱材表面及斷面之掃描式電子顯微鏡(SEM)照片，(c)及(d)為矽膠-矽氣凝膠-矽烷偶合劑氣凝膠/複合非織物防火隔熱材斷面放大照片，由照片中可 證明矽膠-矽氣凝膠-矽烷偶合劑氣凝膠充填於非織物纖維間空隙，並形成多孔性的網狀結構，且矽膠-矽氣凝膠-矽烷偶合劑氣凝膠與非織物纖維之間有極優異的表面結合能力，且非織物與氣凝膠相互之間形成相互穿插的3-D立體網狀結構，顯示利用本發明所製備的矽膠-矽氣凝膠-矽烷偶合劑氣凝膠可與疏水性非織物纖維間形成優異的結合，以增加本產品的使用壽命與提升物理性質。
較佳的是，該鹼觸媒係氫氧化銨NH4OH、氫氧化鈉NaOH、氫氧化鉀KOH、氫氧化鈣Ca(OH)2、碳酸鈉Na2COOH、碳酸氫鈉NaHCOOH及碳酸鈣CaCOOH混合鹼或單一鹼當任鹼觸媒，而該第二含水有機溶液係選自：水、去離子水、C1-C5醇類、C1-C5氨類、C2-C7多醇類或C2-C5酮類所構成群組之一或其組合。在本發明較佳實施例中，該第二含水有機溶液係以水和乙醇溶劑為範例說明。選擇醇類、氨類、多醇類、酮類的目的為視非織物基材的親疏水性質而進行混合比例變化，主要是醇類、氨類、多醇類、酮類等溶劑可相互互溶。
較佳的是，該水解反應時間為10分鐘至60分鐘，該水解反應時間係隨著該酸觸媒的莫耳百分比含量增加而縮短；當該鹼觸媒的莫耳比含量對酸觸媒為1比1 時凝膠化時間約1100分鐘；而鹼觸媒的莫耳比含量對酸觸媒為3比1時凝膠化時間縮短至約3分鐘，藉以控制該非織物含浸加工製程時間。該縮合反應時間係隨著該鹼觸媒的莫耳百分比含量增加而縮短。
較佳的是，該氣凝膠/複合非織物防火隔熱材中所含該氣凝膠的體積百分比含量範圍為百分之20至百分之75。當該氣凝膠的體積百分比含量在35以下時，即能作為一般隔熱材使用，藉此節省該氣凝膠的用量以控制製造成本。當該氣凝膠的體積百分比含量在35以上時，除具有優良隔熱效果外，更能達到防火的效果，以做為建築用防火隔熱材使用。
較佳的是，該乾燥程序之條件為在於室溫下進行自然乾燥，或在攝氏30度至80度，3600分鐘至120分鐘條件下進行快速乾燥，藉此免除習知氣化含水有機溶劑需較高溫度進行，而易導致氣凝膠產生龜裂瓦解的現象，從而提高產品良率。
較佳的是，該複合非織物毯係由聚乙烯(PE)、聚丙烯(PP)、聚乙丙烯(PPE)、聚對苯二甲酸乙二醇酯(PET)或聚醯胺(Nylon)、玻纖、岩棉、碳纖棉其中之一或其組合所製成，不同複合非織物務須配合氣凝膠 體系中矽膠-矽氣凝膠-矽烷偶合劑混合比例，使該複合非織物能與該複合氣凝膠間產生較強結合效果而不易脫落。
惟以上所述者，僅為本發明之較佳實施例而已，當不能以此限定本發明實施之範圍，即大凡依本發明申請專利範圍及發明說明內容所作之簡單的等效變化與修飾，皆仍屬本發明專利涵蓋之範圍內。

Claims (10)

  1. 一種氣凝膠/複合非織物防火隔熱材之製備方法，其包括下列步驟：(1)混合步驟：提供一烷氧化矽類，與一矽膠類進行混合，再添加一矽烷偶合劑類繼續攪拌，其中，該烷氧化矽類：矽膠類：矽烷偶合劑類的莫耳比為1.0：0.0001：0.0001至1.0：0.65：1.0；(2)水解步驟：添加一酸觸媒水溶液於(1)混合步驟之混合溶液中進行一水解反應，過程中再添加矽烷偶合劑水溶液繼續攪拌，以獲得一矽膠-矽氣凝膠-矽烷偶合劑混合之水解溶液，其中，該酸觸媒選自於硫酸H 2SO 4、磷酸H 3PO 4、硝酸HNO 3、鹽酸HCl所構成之一或其組合；(3)縮合步驟：提供一含水鹼觸媒以及含水有機溶液所配置成之一鹼觸媒含水有機溶液，並加入至該水解溶液中，進行一縮合反應，以形成凝膠化之一矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液之縮合溶液，其中，該鹼觸媒選自於NaOH、NaHCO 3、Na 2CO 3、NH 4OH所構成之一或其組合；及(4)成型步驟：取未凝膠化的矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液含浸一回收複合非織物毯或一般非織物毯，使前述矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液充分與非織物完全含浸，並經一乾燥程序，以形成一親水性或疏水性氣凝膠/複合非織物防火隔熱材。
  2. 如申請專利範圍第1項所述氣凝膠/複合非織物防火隔熱材之製備方法，其中，在該混合步驟中，烷氧化矽類與矽膠類的莫耳比為1.0：0.001至1.0：5.0，且該矽膠類為雙末端雙官能基或雙末端加測鏈之叁至肆官能基 之矽膠結構，該矽膠類官能基選自於酸基(-COOH)、胺基(-NH 2)、羥基(-OH)、縮酸基、環氧基、醚基所構成之一或其組合。
  3. 如申請專利範圍第1項所述氣凝膠/複合非織物防火隔熱材之製備方法，其中，在該水解步驟中，該烷氧化矽類：矽膠類：矽烷偶合劑類的莫耳比為1.0：0.01：0.001至1.0：0.65：1.0，該水解溶液中矽膠-矽氣凝膠-矽烷偶合劑與含水有機溶液的體積比為5：95至100：200，該矽烷偶合劑為一含稀烃類或含長鏈稀烃類矽烷結構，且該矽烷偶合劑選自於氯化矽烷偶合劑、稀基矽烷偶合劑、環氧基矽烷偶合劑、酸基矽烷偶合劑、胺基矽烷偶合劑、羥基矽烷偶合劑或縮酸基矽烷偶合劑等。
  4. 如申請專利範圍第1項所述氣凝膠/複合非織物防火隔熱材之製備方法，其中，該鹼觸媒含水有機溶液中鹼觸媒與酸觸媒的莫耳比為1.02比1至3比1，當鹼觸媒的莫耳比越大，該氣凝膠溶液的凝膠化速率越快。
  5. 如申請專利範圍第1項所述氣凝膠/複合非織物防火隔熱材之製備方法，其中，在該成型步驟中，該矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液穿插在該非織物中，且該成型步驟可透過噴塗、淋噴、含浸加工或溶液連續壓吸加工等方式進行實現。
  6. 如申請專利範圍第1項所述氣凝膠/複合非織物防火隔熱材之製備方法，其中，該水解溶液以及該縮合溶液中含水有機溶液的水的莫耳含量為0mol%至80mol%，當溶液中水的莫耳含量小於10mol%可製備表面親水性質的氣凝膠/複合非織物防火隔熱材，當溶液中水的莫耳含量大於10mol%可製備表面疏水性質的氣凝膠/複合非織物防火隔熱材。
  7. 如申請專利範圍第1項所述氣凝膠/複合非織物防火隔熱材之製備方法，其中，該水解溶液以及該縮合溶液中含水有機溶液的水的莫耳含量為0mol%至80mol%，當溶液中水的莫耳含量越高，所製備的氣凝膠/複合非織物防火隔熱材的防火性能越優異。
  8. 如申請專利範圍第1項所述氣凝膠/複合非織物防火隔熱材之製備方法，其中，該水解溶液以及該縮合溶液中含水有機溶液的水的莫耳含量為2.0mol%至80mol%。
  9. 如申請專利範圍第1項所述氣凝膠/非織物防火隔熱材之製備方法，其中，該氣凝膠/複合非織物防火隔熱材中所含該矽膠-矽氣凝膠-矽烷偶合劑氣凝膠的體積百分比含量為百分之5至百分之80。
  10. 如申請專利範圍第1項所述之氣凝膠/非織物複合隔熱材製備方法，其中，在該成型步驟中，該乾燥程序之條件為常溫常壓下進行無水氣凝膠乾燥，或利用攝氏30度至80度間進行有機溶液快速汽化乾燥程序，該非織物係利用聚乙烯(PE)、聚丙烯(PP)、聚乙丙烯(PPE)、聚酯(Polyester)、聚醯胺(Polyamine)、玻璃纖維(glass fiber)、岩棉其中之一或其組合所製成。
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