TWI741746B - Manufacturing method of silica aerogel composite fiber blanket - Google Patents
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Abstract
一種二氧化矽氣凝膠複合纖維毯之製造方法，主要即先製備出一種性能優良的"改質濕矽氣凝膠"，再應用該"改質濕矽氣凝膠"進一步製造出一種高強度、柔曲性佳、耐高溫、絕熱性能佳，且不掉粉的"二氧化矽氣凝膠複合纖維毯"；本發明所製造出的"二氧化矽氣凝膠複合纖維毯"因為低熱傳導率，用來作為隔熱材料能獲致絕佳效果，尤其用來披覆於熱流體管路外壁上做為絕熱層時，可以隔絕流體管路的熱量散失，達致大幅節省能源之功效；同時可以降低所披覆管線壁面之腐蝕，達致節省檢視維修花費之功效。A method for manufacturing silica aerogel composite fiber blanket, which is to first prepare a "modified wet silica aerogel" with excellent performance, and then use the "modified wet silica aerogel" to further produce a high The "silica aerogel composite fiber blanket" has good strength, flexibility, high temperature resistance, and good thermal insulation performance, and does not drop powder; the "silica aerogel composite fiber blanket" manufactured by the present invention is low in Thermal conductivity, used as a thermal insulation material to achieve excellent results, especially when used as a thermal insulation layer on the outer wall of the hot fluid pipeline, it can isolate the heat loss of the fluid pipeline and achieve a significant energy saving effect; At the same time, it can reduce the corrosion of the covered pipeline wall, and achieve the effect of saving inspection and maintenance costs.
Description
本發明係關於一種二氧化矽氣凝膠複合纖維毯之製造方法，尤指一種將二氧化矽氣凝膠與纖維毯複合製造之方法。The invention relates to a method for manufacturing a silica aerogel composite fiber blanket, in particular to a method of composite manufacturing a silica aerogel and a fiber blanket.
按，氣凝膠（aerogels）是指以奈米量級超微顆粒相互聚集構成奈米多孔網狀結構，並在網狀孔隙中充滿氣態分散介質的輕質奈米固態材料。不同氣凝膠的製備方法也不相同，但是其製備歷程大同小異，一般是採用溶膠-凝膠法製備出濕凝膠（wet gel），然後再將濕凝膠經過溶劑置換和超臨界乾燥得到相應的氣凝膠。氣凝膠的特性在於：(a)孔隙率很高；可高達99.8%； (b)奈米級別孔洞(2 ~ 50 nm)和三維奈米骨架顆粒(2 ~ 5 nm)；(c) 高比表面積，可高達1000 m 2/g；(d) 低密度，可低至0.003 g/cm 3；（e）熱導率極低，常溫下可以低至0.013 W/(mK)，比空氣的導熱係數還低；（f）由於其比表面積和孔隙率很高，密度很低，導致其強度低，脆性大。氣凝膠在現代高科技工業範圍內是一種超級絕熱材料，在很多產業上都被運用到。美國史丹福大學的S.S. Kistler首先利用水玻璃通過溶膠-凝膠方法及超臨界乾燥技術製得二氧化矽氣凝膠 (SiO 2aerogels），亦可稱為"矽氣凝膠"。 According to this, aerogels refer to lightweight nano-solid materials in which nano-scale ultrafine particles aggregate with each other to form a nanoporous network structure, and the network pores are filled with a gaseous dispersion medium. Different aerogels have different preparation methods, but their preparation processes are similar. Generally, a wet gel is prepared by a sol-gel method, and then the wet gel is subjected to solvent replacement and supercritical drying to obtain the corresponding Of aerogel. The characteristics of aerogels are: (a) high porosity; up to 99.8%; (b) nano-scale pores (2 ~ 50 nm) and three-dimensional nano-frame particles (2 ~ 5 nm); (c) high The specific surface area can be as high as 1000 m 2 /g; (d) low density can be as low as 0.003 g/cm 3 ; (e) thermal conductivity is extremely low, which can be as low as 0.013 W/(mK) at room temperature, which is higher than that of air The thermal conductivity is still low; (f) Because of its high specific surface area and porosity, and low density, it has low strength and high brittleness. Aerogel is a kind of super thermal insulation material in the modern high-tech industry, and it is used in many industries. SS Kistler of Stanford University in the United States first used water glass to prepare silica aerogels (SiO 2 aerogels) through the sol-gel method and supercritical drying technology, which can also be called "silica aerogels."
二氧化矽氣凝膠之製備在各國已有多件專利存在於先前，其中皆必須經過｢置換｣及｢改質｣二道作業，且不論｢置換｣或｢改質｣或｢置換+改質｣，都是採行"容器浸置"方法進行，亦即準備一適當容積之反應容器，可為密閉式或不完全密閉式，端視有機溶劑性質而定，然後將濕凝膠置放於該反應容器內，再注入選定之適當溶劑或改質劑，以進行預期之｢置換｣及｢改質｣作業，其中｢置換｣作業尤為重要，因為採行"容器浸置"方法進行｢置換｣作業時，反應時間較長，且會使用到大量的溶劑，故針對｢置換｣作業，本發明人已研發一種可以減縮濕凝膠溶劑置換作業時間，且得以大幅提升置換效果之二氧化矽氣凝膠之製備方法，並已提出台灣第109106708號「二氧化矽氣凝膠之製備方法」發明專利申請案及中國第202010142667.0「二氧化矽氣凝膠之製備方法」發明專利申請案。There have been many patents for the preparation of silica aerogel in various countries, and all of them must go through two operations of "replacement" and "modification", regardless of "replacement" or "modification" or "replacement + modification". The quality is all carried out by the "container immersion" method, that is, prepare a reaction container of appropriate volume, which can be closed or incompletely closed, depending on the nature of the organic solvent, and then place the wet gel Into the reaction vessel, inject the selected appropriate solvent or modifier to perform the expected "replacement" and "modification" operations. The "replacement" operation is particularly important because the "container immersion" method is adopted. During the replacement operation, the reaction time is longer and a large amount of solvents are used. Therefore, for the replacement operation, the inventors have developed a kind of dioxide that can reduce the time of the wet gel solvent replacement operation and greatly improve the replacement effect. For the preparation method of silica aerogel, Taiwan has filed Taiwan No. 109106708 "Silica aerogel preparation method" invention patent application and China No. 202010142667.0 "Silica aerogel preparation method" invention patent application.
本發明人完成上述「二氧化矽氣凝膠之製備方法」專利之研發後，遂進一步針對二氧化矽氣凝膠之後端應用進行研究改良，在眾多應用產品中，發明人注意到"氣凝膠複合纖維毯"產品之製造值得研究創新。"氣凝膠複合纖維毯" 係一種將"氣凝膠"與"複合纖維毯"加以結合而成之產品，主要具有耐高溫、絕熱性能佳之特點，進而可以降低絕熱層覆蓋下方腐蝕之可能性，因此適用於做為絕熱耐火及防腐蝕之材料，經常被使用於流體管線外部覆蓋做為絕熱層，以大幅降低管線內部熱量之流失(節省能源花費)，同時也可大幅阻絕管線外部之腐蝕(節省檢視維修花費)。After the inventor completed the research and development of the above-mentioned "method for preparing silica aerogel", he further researched and improved the back-end application of silica aerogel. Among many applications, the inventor noticed that "aerosol The manufacture of "rubber composite fiber blanket" is worthy of research and innovation. "Aerogel composite fiber blanket" is a product that combines "aerogel" and "composite fiber blanket". It mainly has the characteristics of high temperature resistance and good thermal insulation performance, which can reduce the possibility of corrosion under the insulation layer. Therefore, it is suitable as a heat-insulating, fire-resistant and anti-corrosion material. It is often used as an insulation layer for the outer covering of fluid pipelines to greatly reduce the heat loss inside the pipeline (saving energy costs), and it can also greatly prevent corrosion outside the pipeline (Save inspection and maintenance costs).
關於"氣凝膠複合纖維毯"之製造方面已有多件專利存在於先前，舉例有： 1.TW I535658｢非織物/氣凝膠複合防火/隔熱材及其製備方法｣台灣發明專利，係先經過一水解步驟及一縮合步驟製備出一氣凝膠，然後在成型步驟時取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，以形成一非織物/氣凝膠複防火/隔熱材，其中，將氣凝膠充分穿插在該非織物中係透過含浸加工方式或連續滾壓方式實現；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。總結而言，TW I535658案係採將製得之氣凝膠穿插在非織物中加以乾燥之直接製備法。 2.TW I643888｢氣凝膠／複合非織物防火隔熱材之製備方法｣台灣發明專利，係先經過一混合步驟、一水解步驟及一縮合步驟，以形成一未凝膠化之矽膠-矽氣凝膠-矽烷偶合劑氣凝膠溶液之縮合溶液，然後在成型步驟時採含浸、噴塗、淋噴、或溶液連續壓吸該未凝膠化的矽膠-矽 氣凝膠-矽烷偶合劑氣凝膠溶液之縮合溶液至一回收複合非織物毯或一般非織物毯，使該 矽膠-矽氣凝膠-矽烷偶合劑氣凝膠凝膠化並穿插在該非織物毯中，並經一乾燥程序，以形成一氣凝膠/複合非織物防火隔熱材，其中，該乾燥程序之條件為常溫常壓下進行氣凝膠乾燥，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，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。總結而言，TW I643888案係採將未凝膠化的矽膠-矽 氣凝膠-矽烷偶合劑氣凝膠溶液之縮合溶液穿插在回收複合非織物毯或一般非織物毯中加以乾燥之直接製備法。 3.TW I663062｢氣凝膠複合體及其製備方法｣台灣發明專利，其係濕潤包括無機纖維及有機纖維中之至少一者的一纖維材料；以一卷形式捲取該經濕潤之纖維材料與一隔片或以一平面形式積層該經濕潤之纖維材料與該隔片；將該纖維材料饋進一容器內；藉將一前驅物注入該容器內及膠凝該前驅物同時於真空下去除殘餘氣泡而製備一凝膠-纖維複合物；自該容器取出 該凝膠-纖維複合物及去除該隔片；溶劑取代及有機表面改性該凝膠-纖維複合物；及大氣壓乾燥及超臨界乾燥該經有機表面改性的凝膠-纖維複合物。總結而言，TW I663062案係將凝膠藉一前驅物注入纖維材料內，再行溶劑取代及有機表面改性，及大氣壓乾燥及超臨界乾燥之直接製備法。 4.KR 101786283 B1｢氣凝膠毯和生產方法｣韓國發明專利，係將二氧化矽氣凝膠、聚合物膠乳乳液、黏結劑、漿料、纖維、橡皮布之材料採漿料浸泡法，使矽酸、聚合物膠乳乳液、黏結劑及漿料混合為矽酸凝膠，並使纖維充分含浸後黏結於橡皮布上成為膠毯。 5.CN 104496403 B｢一種增強型氣凝膠複合材料｣中國發明專利，係在二氧化矽氣凝膠塊體的表面或塊體界面之間，通過纖維網格布增強的水性膠黏劑包覆或黏結成一體，總結而言，CN 104496403 B係採黏結法，使二氧化矽氣凝膠塊體與纖維網格布黏結成一體。 6.US 6770584 B2｢混合氣凝膠硬質陶瓷纖維絕緣材料及其製造方法(Hybrid aerogel rigid ceramic fiber insulation and method of producing same)｣美國發明專利，主要係訴求一種絕緣材料，包括：由燒結陶瓷纖維形成的多孔基材，其中所述陶瓷纖維包含60 ~ 80 wt. ％的二氧化矽纖維、20 ~ 40 wt. ％的氧化鋁纖維及 0.1 ~ 1.0 wt. ％的含硼成分；以及一納米多孔材料，浸漬在所述多孔基材中。US6770584B2同時訴求一種生產絕緣材料的方法，包括：形成混合陶瓷纖維的水性漿料，其中所述纖維包含60 ~ 80 wt. ％的二氧化矽纖維、20 ~ 40 wt. ％的氧化鋁纖維及 0.1 ~ 1.0 wt. ％的含硼成分；從漿液中除去至少一部分水；將陶瓷纖維壓成濕的坯料；從濕的坯料上去除殘留的水；將陶瓷纖維彼此熔合以形成多孔基材。 並且用氣凝膠材料浸漬多孔質基材。總結而言，US 6770584 B2係採將氣凝膠材料浸漬多孔質基材之直接製備法。 There have been many patents on the manufacture of "aerogel composite fiber blanket". Examples include: 1. TW I535658 “Non-woven/aerogel composite fireproof/heat insulation material and its preparation method” Taiwan invention patent, is to prepare an aerogel through a hydrolysis step and a condensation step, and then take the aforementioned gas during the forming step The gel is added to a non-woven fabric, the aforementioned aerogel is fully inserted into the non-woven fabric, and a drying process is performed to form a non-woven/aerogel composite fire/heat insulation material, wherein the aerogel is fully inserted In the non-woven fabric, it is achieved through impregnation processing or continuous rolling; the conditions of the drying process are anhydrous aerogel drying at normal temperature and pressure, or a rapid vaporization and drying process of organic solution at 30 to 80 degrees Celsius. In summary, the TW I535658 case adopts a direct preparation method in which the prepared aerogel is interspersed in a non-woven fabric and dried. 2. TW I643888 "Aerogel/Composite Non-woven Fireproof Thermal Insulation Material Preparation Method" Taiwan invention patent, it first goes through a mixing step, a hydrolysis step and a condensation step to form an ungelled silicone-silicone The condensation solution of aerogel-silane coupling agent aerogel solution is then impregnated, sprayed, sprayed, or the solution is continuously pressed to suck the ungelled silica gel-silicon aerogel-silane coupling agent gas during the forming step The condensation solution of the gel solution is transferred to a recycled composite non-woven blanket or general non-woven blanket, so that the silica gel-silicon aerogel-silane coupling agent aerogel is gelled and interspersed in the non-woven blanket, and undergoes a drying process , To form an aerogel/composite non-woven fire-proof insulation material, wherein the conditions of the drying process are aerogel drying at room temperature and pressure, or a rapid vaporization and drying process of organic solution at 30°C to 80°C. The non-woven fabric is made of polyethylene (PE), polypropylene (PP), polyethylene propylene (PPE), polyester (Polyester), polyamine (Polyamine), glass fiber (glass fiber), rock wool or one of them The combination is made. In summary, the TW I643888 case is a direct preparation by interspersing the condensation solution of the ungelled silica gel-silica aerogel-silane coupling agent aerogel solution in a recycled composite non-woven blanket or general non-woven blanket and drying it. Law. 3. TW I663062 "Aerogel composite and its preparation method" Taiwan invention patent, which moistens a fibrous material including at least one of inorganic fiber and organic fiber; winds up the moistened fibrous material in the form of a roll Laminate the wetted fibrous material and the spacer with a separator or in a flat form; feed the fibrous material into a container; simultaneously remove under vacuum by injecting a precursor into the container and gelling the precursor Residual bubbles to prepare a gel-fiber composite; take out the gel-fiber composite from the container and remove the spacer; solvent replacement and organic surface modification of the gel-fiber composite; and atmospheric pressure drying and supercritical The organic surface-modified gel-fiber composite is dried. In summary, the TW I663062 case is a direct preparation method of injecting the gel into the fiber material with a precursor, then performing solvent substitution and organic surface modification, as well as atmospheric pressure drying and supercritical drying. 4. KR 101786283 B1 "Aerogel blanket and production method" Korean invention patent, is the slurry soaking method for silica aerogel, polymer latex emulsion, binder, slurry, fiber and blanket. Mix silicic acid, polymer latex emulsion, bonding agent and slurry into silicic acid gel, and make the fiber fully impregnated and bonded to the blanket to form a rubber blanket. 5. CN 104496403 B "A reinforced aerogel composite material" Chinese invention patent, is a water-based adhesive package reinforced by fiber mesh on the surface of silica aerogel block or between the block interface. In summary, CN 104496403 B series adopts the bonding method to bond the silica aerogel block and the fiber mesh cloth into one body. 6.US 6770584 B2 "Hybrid aerogel rigid ceramic fiber insulation and method of producing same)" American invention patent, mainly seeking an insulating material, including: sintered ceramic fiber The formed porous substrate, wherein the ceramic fiber includes 60 ~ 80 wt.% of silica fiber, 20 ~ 40 wt.% of alumina fiber, and 0.1 ~ 1.0 wt.% of boron-containing component; and a nanoporous Material, impregnated in the porous substrate. US6770584B2 also claims a method for producing insulating materials, including: forming an aqueous slurry of mixed ceramic fibers, wherein the fibers include 60 ~ 80 wt.% silica fiber, 20 ~ 40 wt.% alumina fiber and 0.1 ~ 1.0 wt.% of boron content; remove at least part of the water from the slurry; press the ceramic fibers into a wet blank; remove residual water from the wet blank; fuse the ceramic fibers with each other to form a porous substrate. And the porous base material is impregnated with the aerogel material. In summary, US 6770584 B2 adopts a direct preparation method of impregnating aerogel material with a porous substrate.
上述 TW I535658、TW I643888、TW I663062、KR 101786283 B1、CN 104496403 B、US 6770584 B2專利雖皆係關於氣凝膠複合纖維毯或隔熱材的製造，然有的是採直接製備法，有的則是採不同材料的漿料浸泡法，以及有的是採黏結法，結果都存在著氣凝膠容易自纖維毯上掉落之缺失，一般俗稱為"掉粉"。當氣凝膠複合纖維毯上容易掉粉時，就等於其耐高溫之效果及絕熱性能顯屬不佳，很明顯就導致其使用期限大幅縮減，此為最大缺失。再者，上述諸案對於訴求專利之氣凝膠複合纖維毯或隔熱材，在強度或柔軟性的改善方面，於專利說明書中並未述及有明確驗證，致其實用進步性難以理解。Although the above-mentioned patents TW I535658, TW I643888, TW I663062, KR 101786283 B1, CN 104496403 B, and US 6770584 B2 are all related to the manufacture of aerogel composite fiber blankets or thermal insulation materials, some are directly prepared, and some are The slurry soaking method of different materials, and some of the bonding method, the result is that there is a lack of aerogel easily falling from the fiber blanket, which is generally called "powdering". When the powder on the aerogel composite fiber blanket is easy to fall off, it means that its high temperature resistance and thermal insulation performance are not good, which obviously leads to a significant reduction in its service life, which is the biggest deficiency. Furthermore, in the above-mentioned cases, the improvement of the strength or flexibility of the aerogel composite fiber blanket or thermal insulation material for which the patent is claimed is not clearly verified in the patent specification, which makes it difficult to understand the practical progress.
針對上述先前技術之若干缺失，本發明人萌生改良之發想，並即深入構思研發創作，經長時間努力，終有本發明產生。In view of the above-mentioned shortcomings of the prior art, the present inventors have developed ideas for improvement, and in-depth conception, research, development and creation. After a long period of hard work, the present invention is finally produced.
緣是，本發明之主要目的即在提供一種可以製造出高強度、柔曲性佳、耐高溫、絕熱性能佳之二氧化矽氣凝膠複合纖維毯之製造方法。The reason is that the main purpose of the present invention is to provide a method for manufacturing a silica aerogel composite fiber blanket with high strength, good flexibility, high temperature resistance, and good thermal insulation performance.
本發明之另一主要目的則在提供一種特別適用於流體管線外部覆蓋做為絕熱層，以降低管線內熱量流失及降低管線壁面腐蝕之二氧化矽氣凝膠複合纖維毯之製造方法。Another main purpose of the present invention is to provide a method for manufacturing a silica aerogel composite fiber blanket that is particularly suitable for covering the exterior of fluid pipelines as a thermal insulation layer to reduce heat loss in the pipeline and reduce corrosion of the pipeline wall.
為達成上述目的，本發明特別設計一種二氧化矽氣凝膠複合纖維毯之製造方法 ，係經過如下步驟： (1). 將模數為2.53 ~ 3.33的矽酸鈉及去離子水配置成固含量6 ~ 12.5 wt. %的矽酸鈉溶液並攪拌均勻； (2). 將上述矽酸鈉溶液加入H+離子交換樹脂進行水解反應，得到酸鹼值pH: 2 ~ 3的矽酸溶液，然後將H+離子交換樹脂過濾去除(所過濾去除的H+離子交換樹脂可再生使用)； (3). 將鹼性催化劑添加入上述矽酸鈉溶液內進行縮合反應，以得到濕凝膠； (4). 將上述濕凝膠置於攪拌機中，加入異丙醇溶劑，然後在溫度25 ~ 80℃下，以50 rpm攪拌老化1 ~ 12小時； (5). 將經老化後之濕凝膠加入異丙醇與正己烷之混合溶液，然後在溫度25 ~ 80℃下，以500 rpm攪拌進行溶劑連續循環過濾置換1 ~ 12小時，置換後再以抽氣過濾去除異丙醇與正己烷之混合溶液； (6). 加入改質劑六甲基二矽氮烷與正己烷溶劑之混合溶液，矽烷改質劑與矽酸莫耳比為 1：0.35 ~ 1.67，在溫度25 - 80℃下，以500 rpm攪拌進行表面疏水化改質1 - 12小時，反應結束後以正己烷溶劑清洗過濾去除未反應的矽氧烷改質劑，當完成改質後將濕凝膠與溶液分離，此時的濕凝膠為經過疏水化改質的改質濕矽氣凝膠； (7).將 1 ~ 5 wt.% 黏結劑、1 ~ 5 wt.% 改質濕矽氣凝膠及0.05 ~ 0.5 wt.%增稠劑添加於50 ~ 120 mL的純水裡，在30 ~ 70℃下以200 ~ 800 rpm 攪拌10 ~ 60分鐘，配置成為一黏著劑漿料；該黏結劑係由一有機黏結劑及一無機黏結劑所混合組成，該有機黏結劑可係聚乙烯醇及丙烯酸乳液其中之一種，該無機黏結劑為蒙脫石，所以該黏結劑可以是由丙烯酸乳液與蒙脫石混合組成，也可以是由聚乙烯醇與蒙脫石混合組成；該增稠劑為一種纖維素，可係十二烷基苯磺酸鈉界面活性劑、氟化改質丙烯酸界面活性劑、羥丙基纖維素及羥乙基纖維素其中之一種； (8).將上述配置之黏著劑漿料加入改質劑，該改質劑重量比為1 ~ 6 wt.%，該改質劑可係六甲基二矽氮烷、甲基三甲氧基矽烷、苯基三甲基矽烷及聚二甲基矽氧烷其中之一種，該改質劑具有偶合劑及表面改質劑之作用效果； (9).將經過改質之黏著劑漿料浸泡於玻璃纖維毯中，在40 ~ 80℃下進行交聯反應及產生螯合作用0.5 ~ 3小時，成為一濕性的二氧化矽氣凝膠複合纖維毯； (10).將經過交聯反應及螯合作用後處於濕性的二氧化矽氣凝膠複合纖維毯，在100℃中進行乾燥5小時，成為一乾性的二氧化矽氣凝膠複合纖維毯。 In order to achieve the above objective, the present invention specifically designs a manufacturing method of silica aerogel composite fiber blanket, which goes through the following steps: (1). Prepare sodium silicate with a modulus of 2.53 ~ 3.33 and deionized water into a sodium silicate solution with a solid content of 6 ~ 12.5 wt.% and stir it evenly; (2). Add the above sodium silicate solution to H+ ion exchange resin for hydrolysis to obtain a silicic acid solution with an acid-base value of pH: 2 ~ 3. Then filter the H+ ion exchange resin to remove (the filtered H+ ion exchange resin Renewable use); (3) Add an alkaline catalyst to the above sodium silicate solution for condensation reaction to obtain a wet gel; (4). Put the above wet gel in a mixer, add isopropanol solvent, and then stir and age at 50 rpm for 1 to 12 hours at a temperature of 25 to 80°C; (5). Add the aging wet gel to the mixed solution of isopropanol and n-hexane, and then stir at 500 rpm at a temperature of 25 ~ 80 ℃ to perform continuous cycle filtration and replacement of the solvent for 1 ~ 12 hours, and then replace it again. Remove the mixed solution of isopropanol and n-hexane by suction filtration; (6). Add the mixed solution of modifier hexamethyldisilazane and n-hexane solvent, the molar ratio of modifier of silane modifier to silicate is 1:0.35 ~ 1.67, at a temperature of 25-80 ℃, 500 The surface is hydrophobized and modified by stirring at rpm for 1-12 hours. After the reaction is completed, the unreacted silicone modifier is removed by washing and filtering with n-hexane solvent. When the modification is completed, the wet gel is separated from the solution. The gel is a modified wet silica aerogel that has been hydrophobized and modified; (7). Add 1 ~ 5 wt.% binder, 1 ~ 5 wt.% modified wet silica aerogel, and 0.05 ~ 0.5 wt.% thickener to 50 ~ 120 mL of pure water, and add 30 to 30 mL of pure water. Stir at 200-800 rpm at ~70°C for 10-60 minutes to form an adhesive slurry; the adhesive is a mixture of an organic adhesive and an inorganic adhesive. The organic adhesive can be polyvinyl alcohol One of acrylic emulsion and acrylic emulsion, the inorganic binder is montmorillonite, so the adhesive can be composed of acrylic emulsion mixed with montmorillonite, or it can be composed of polyvinyl alcohol and montmorillonite; the thickener It is a kind of cellulose, which can be one of sodium dodecylbenzene sulfonate surfactant, fluorinated modified acrylic surfactant, hydroxypropyl cellulose and hydroxyethyl cellulose; (8). Add the adhesive slurry of the above configuration to the modifier, the modifier weight ratio is 1 ~ 6 wt.%, the modifier can be hexamethyldisilazane, methyltrimethoxy One of silane, phenyltrimethylsilane and polydimethylsiloxane, the modifier has the effect of coupling agent and surface modifier; (9). Soak the modified adhesive slurry in a glass fiber blanket, and carry out cross-linking reaction and chelation at 40 ~ 80 ℃ for 0.5 ~ 3 hours to become a wet silica vapor condensation Glue composite fiber blanket; (10). After the cross-linking reaction and chelation, the silica aerogel composite fiber blanket that is wet is dried at 100°C for 5 hours to become a dry silica aerogel composite fiber blanket .
上述之二氧化矽氣凝膠複合纖維毯之製造方法，步驟(2)中優選為將矽酸鈉溶液加入H+離子交換樹脂進行水解反應，得到酸鹼值pH: 2.4 ~ 2.6的矽酸溶液。In the above-mentioned manufacturing method of silica aerogel composite fiber blanket, in step (2), it is preferable to add sodium silicate solution to H+ ion exchange resin for hydrolysis reaction to obtain a silicic acid solution with an acid-base value of pH: 2.4-2.6.
上述之二氧化矽氣凝膠複合纖維毯之製造方法，步驟(3)中優選為該鹼性催化劑係氫氧化銨，並以加入1M鹼性催化劑直至矽酸鈉溶的酸鹼值升至pH: 4 ~ 7進行縮合反應以得到濕凝膠。In the above-mentioned manufacturing method of silica aerogel composite fiber blanket, in step (3), the alkaline catalyst is preferably ammonium hydroxide, and 1M alkaline catalyst is added until the acid-base value dissolved in sodium silicate rises to pH : 4 ~ 7 conduct condensation reaction to get wet gel.
上述之二氧化矽氣凝膠複合纖維毯之製造方法，步驟(4)中所加入異丙醇溶劑與濕凝膠之體積比為1：1；以及步驟(5)中所加入異丙醇與正己烷之混合溶液與濕凝膠體積比為 1：1。In the above-mentioned manufacturing method of silica aerogel composite fiber blanket, the volume ratio of the isopropanol solvent and the wet gel added in step (4) is 1:1; and the isopropanol and the wet gel added in step (5) The volume ratio of the mixed solution of n-hexane to the wet gel is 1:1.
上述之二氧化矽氣凝膠複合纖維毯之製造方法，步驟(6)中優選為矽烷改質劑與矽酸莫耳比為 1：1.15，在溫度80℃下，以500 rpm攪拌進行表面疏水化改質6小時。In the manufacturing method of the above-mentioned silica aerogel composite fiber blanket, in step (6), it is preferable that the molar ratio of silane modifier and silicate is 1:1.15, and the surface is hydrophobicized by stirring at a temperature of 80°C at 500 rpm. Chemical modification for 6 hours.
上述之二氧化矽氣凝膠複合纖維毯之製造方法，步驟(7)中優選為將2 wt.% 黏結劑、1 wt.% 改質濕矽氣凝膠及0.25 wt. %增稠劑添加於100 mL的純水裡，在50℃下以500 rpm 攪拌30分鐘，配置成為一黏著劑漿料。In the above-mentioned manufacturing method of silica aerogel composite fiber blanket, in step (7), it is preferable to add 2 wt.% binder, 1 wt.% modified wet silica aerogel and 0.25 wt.% thickener In 100 mL of pure water, stir at 500 rpm at 50°C for 30 minutes to prepare an adhesive slurry.
上述之二氧化矽氣凝膠複合纖維毯之製造方法，步驟(7)中優選為該有機黏結劑與該無機黏結劑之重量比為1：1。In the manufacturing method of the above-mentioned silica aerogel composite fiber blanket, in step (7), it is preferable that the weight ratio of the organic binder to the inorganic binder is 1:1.
上述之二氧化矽氣凝膠複合纖維毯之製造方法，步驟(8)中優選為該改質劑為六甲基二矽氮烷，重量比3 wt. %。In the manufacturing method of the above-mentioned silica aerogel composite fiber blanket, in step (8), it is preferable that the modifier is hexamethyldisilazane, and the weight ratio is 3 wt.%.
上述之二氧化矽氣凝膠複合纖維毯之製造方法，步驟(9)中優選為進行交聯反應並產生螯合作用時間1小時；以及該玻璃纖維毯為10 x 10 x 0.6 cm。In the above-mentioned manufacturing method of the silica aerogel composite fiber blanket, in step (9), it is preferable to perform a cross-linking reaction and generate a chelation time of 1 hour; and the glass fiber blanket is 10 x 10 x 0.6 cm.
上述之二氧化矽氣凝膠複合纖維毯之製造方法，步驟(9)或步驟(10)中優選為該玻璃纖維毯係玻璃纖維棉毯或玻璃纖維針軋毯。In the manufacturing method of the above-mentioned silica aerogel composite fiber blanket, in step (9) or step (10), it is preferable that the glass fiber blanket is a glass fiber cotton blanket or a glass fiber needled blanket.
關於本發明為達成上述目的，所採用之技術手段及可達致之功效，茲舉以下較佳可行實施例配合附圖進行詳細解說說明，俾利完全瞭解。With regard to the technical means adopted and the achievable effects of the present invention in order to achieve the above-mentioned objects, the following preferred and feasible embodiments are described in detail with the accompanying drawings for a complete understanding of the benefits.
本發明主要係訴求一種二氧化矽氣凝膠複合纖維毯之製造方法，因此必須於前端先製備出二氧化矽氣凝膠，然後再將所製得之二氧化矽氣凝膠應用於後端製造出複合纖維毯。The present invention mainly seeks a method for manufacturing silica aerogel composite fiber blanket. Therefore, it is necessary to prepare silica aerogel at the front end, and then apply the prepared silica aerogel to the back end Manufactured composite fiber blanket.
請參閱圖1所示，本發明於前端製備出二氧化矽氣凝膠，係經過如下步驟：
(1). 將模數為2.53 ~ 3.33的矽酸鈉及去離子水配置成固含量6 ~ 12.5 wt. %的矽酸鈉溶液並攪拌均勻。
(2). 將上述矽酸鈉溶液加入 H+離子交換樹脂進行水解反應，得到酸鹼值pH: 2 ~ 3的矽酸溶液，優選為得到酸鹼值pH: 2.4 ~ 2.6的矽酸溶液，然後將H+離子交換樹脂過濾去除，至於所過濾去除的H+離子交換樹脂係可再生使用。
(3). 接著將鹼性催化劑添加入上述矽酸鈉溶液內進行縮合反應，以得到濕凝膠，優選為該鹼性催化劑係氫氧化銨，並以加入1M鹼性催化劑直至矽酸鈉溶的酸鹼值升至pH: 4 ~ 7進行縮合反應以得到濕凝膠。
(4). 將上述濕凝膠置於攪拌機中，加入異丙醇溶劑，優選為所加入異丙醇溶劑與濕凝膠之體積比為1：1；然後在溫度25 ~ 80℃下，以50 rpm攪拌老化1 - 12小時，優選為溫度80℃下，以50 rpm攪拌老化3小時。
(5). 接著將經老化後之濕凝膠加入異丙醇與正己烷之混合溶液，優選為所加入異丙醇與正己烷之混合溶液與濕凝膠體積比為 1：1，然後在溫度25 - 80℃下，以500 rpm攪拌進行溶劑連續循環過濾置換1 - 12小時，優選為連續循環過濾置換6小時後再以抽氣過濾去除異丙醇與正己烷之混合溶液，重複抽氣過濾步驟3 ~ 4次後。
(6). 接著加入改質劑六甲基二矽氮烷與正己烷溶劑之混合溶液，矽烷改質劑與矽酸莫耳比為 1：0.35 ~ 1.67，在溫度25 - 80℃下，以500 rpm攪拌進行表面疏水化改質1 - 12小時，優選為矽烷改質劑與矽酸莫耳比為 1：1.15，在溫度80℃下，以500 rpm攪拌進行表面疏水化改質6小時，反應結束後以正己烷溶劑清洗過濾去除未反應的矽氧烷改質劑，當完成改質後將濕凝膠與溶液分離，這時候的濕凝膠即是業已經過疏水化改質的"疏水性濕二氧化矽氣凝膠"，或即稱"改質濕矽氣凝膠"。
Please refer to Fig. 1, the present invention prepares silica aerogel at the front end, and goes through the following steps:
(1). Prepare sodium silicate with a modulus of 2.53 ~ 3.33 and deionized water into a sodium silicate solution with a solid content of 6 ~ 12.5 wt.% and stir it evenly.
(2). Add the above sodium silicate solution to H+ ion exchange resin for hydrolysis to obtain a silicic acid solution with a pH of 2 to 3, preferably a silicic acid solution with a pH of 2.4 to 2.6, and then The H+ ion exchange resin is filtered and removed, and the filtered H+ ion exchange resin can be reused.
(3). Next, a basic catalyst is added to the above sodium silicate solution for condensation reaction to obtain a wet gel, preferably the basic catalyst is ammonium hydroxide, and a 1M basic catalyst is added until the sodium silicate is dissolved The acid-base value is increased to pH: 4 ~ 7 for condensation reaction to obtain a wet gel.
(4). Put the above wet gel in a mixer, add isopropanol solvent, preferably the volume ratio of the added isopropanol solvent to wet gel is 1:1; then at a temperature of 25 ~ 80 ℃, Stir and age at 50 rpm for 1-12 hours, preferably at a temperature of 80°C, stir and age at 50 rpm for 3 hours.
(5). Then add the aged wet gel to the mixed solution of isopropanol and n-hexane, preferably the volume ratio of the added mixed solution of isopropanol and n-hexane to the wet gel is 1:1, and then At a temperature of 25-80 ℃, stirring at 500 rpm for continuous circulation filtration and replacement of the solvent for 1-12 hours, preferably continuous circulation filtration and replacement for 6 hours, followed by suction filtration to remove the mixed solution of isopropanol and n-hexane, and repeated suction After filtering
因為本發明要進行"二氧化矽氣凝膠複合纖維毯"之製造時，會將該矽氣凝膠與一黏結劑、一增稠劑及一純水共同攪拌混合成為一黏著劑漿料，因此所選用的矽氣凝膠就以上述步驟(6).所完成的"改質濕矽氣凝膠"(即不須經過常壓乾燥者)使用，以節省熱能成本。Because the present invention is to manufacture the "silica aerogel composite fiber blanket", the silica aerogel will be stirred and mixed with a binder, a thickener and a pure water to form a binder slurry. Therefore, the selected silica aerogel is used as the "modified wet silica aerogel" completed in the above step (6) (that is, the one that does not need to be dried under normal pressure) to save heat energy costs.
接著，請參閱圖2所示，要利用上述"改質濕矽氣凝膠"應用於後端製造出複合纖維毯，係經過如下步驟： (1).首先要製備出一黏著劑漿料，其係將 1 ~ 5 wt.%黏結劑(Adhesive)、1 ~ 5 wt.%改質濕矽氣凝膠及0.05 ~ 0.5 wt.%增稠劑添加於50 - 120 mL的純水裡，在30 - 70℃下以200 ~ 800 rpm 攪拌10 ~ 60分鐘，優選為將3 wt.% 黏結劑、1 wt.% 改質濕矽氣凝膠及0.25 wt. %增稠劑添加於100 mL的純水裡，在50℃下以500 rpm 攪拌30分鐘，藉以共同配置成為一黏著劑漿料；其中，該黏結劑係由一有機黏結劑及一無機黏結劑所混合組成，該有機黏結劑與該無機黏結劑之重量比為1：1，該有機黏結劑可係聚乙烯醇(PVA)及丙烯酸乳液(Acrylic emulsion)其中之一種，該無機黏結劑則為蒙脫石(Montmorillonite)，所以該黏結劑可以是由丙烯酸乳液(Acrylic emulsion)與蒙脫石(Montmorillonite)混合組成，也可以是由聚乙烯醇(PVA)與蒙脫石(Montmorillonite)混合組成；該增稠劑為一種纖維素，可係十二烷基苯磺酸鈉界面活性劑、氟化改質丙烯酸界面活性劑、羥丙基纖維素及羥乙基纖維素其中之一種。 (2).將上述配置之黏著劑漿料加入改質劑，該改質劑重量比為1 ~ 6 wt.%，該改質劑可係六甲基二矽氮烷、甲基三甲氧基矽烷、苯基三甲基矽烷及聚二甲基矽氧烷其中之一種，該改質劑具有偶合劑及表面改質劑之作用效果。 (3).將經過改質之黏著劑漿料浸泡於10 x 10 x 0.6 cm的玻璃纖維毯中，在40 ~ 80℃下進行交聯反應並產生螯合作用 0.5 ~ 3小時，就成為一濕性的二氧化矽氣凝膠複合纖維毯，其中，該玻璃纖維毯可係玻璃纖維棉毯或玻璃纖維針軋毯。 (4).最後將經過交聯反應及螯合作用後，處於濕性的二氧化矽氣凝膠複合纖維毯，在100℃中進行乾燥5小時，最後就成為一乾性的二氧化矽氣凝膠複合纖維毯。 Next, please refer to Figure 2. To use the above-mentioned "modified wet silica aerogel" to be applied to the back end to produce a composite fiber blanket, the following steps are required: (1). Firstly, an adhesive slurry must be prepared, which is 1 ~ 5 wt.% adhesive (Adhesive), 1 ~ 5 wt.% modified wet silica aerogel and 0.05 ~ 0.5 wt.% increase The thickener is added to 50-120 mL of pure water, and stirred at 200-800 rpm at 30-70°C for 10-60 minutes, preferably 3 wt.% binder and 1 wt.% modified wet silicon gas are condensed Glue and 0.25 wt.% thickener were added to 100 mL of pure water, and stirred at 500 rpm at 50°C for 30 minutes to form an adhesive slurry together; among them, the adhesive is an organic adhesive And an inorganic binder, the weight ratio of the organic binder to the inorganic binder is 1:1, the organic binder can be one of polyvinyl alcohol (PVA) and acrylic emulsion (Acrylic emulsion), the The inorganic binder is Montmorillonite, so the binder can be composed of acrylic emulsion (Acrylic emulsion) and montmorillonite (Montmorillonite) mixed, or it can be composed of polyvinyl alcohol (PVA) and montmorillonite ( Montmorillonite) mixed composition; the thickener is a cellulose, which can be one of sodium dodecylbenzene sulfonate surfactants, fluorinated modified acrylic surfactants, hydroxypropyl cellulose and hydroxyethyl cellulose A sort of. (2). Add the adhesive slurry of the above configuration to the modifier, the modifier weight ratio is 1 ~ 6 wt.%, the modifier can be hexamethyldisilazane, methyltrimethoxy One of silane, phenyltrimethylsilane and polydimethylsiloxane, the modifier has the effects of coupling agent and surface modifier. (3). Immerse the modified adhesive slurry in a 10 x 10 x 0.6 cm glass fiber blanket, and carry out the cross-linking reaction at 40 ~ 80 ℃ and produce chelation for 0.5 ~ 3 hours. A wet silica aerogel composite fiber blanket, wherein the glass fiber blanket can be a glass fiber cotton blanket or a glass fiber needled blanket. (4). Finally, after cross-linking reaction and chelation, the wet silica aerogel composite fiber blanket is dried at 100°C for 5 hours, and finally becomes a dry silica aerogel Glue composite fiber blanket.
以上係區分成二段步驟進行詳細說明，然實際實施時，可仍選擇區分成二段製作，惟也不排除可以直接連貫製作，在「發明內容」及「發明申請專利範圍」中即皆以連貫步驟做界定。The above is divided into two steps for detailed description. However, in actual implementation, you can still choose to divide into two stages to make, but it does not rule out that you can make directly and coherently. Define consecutive steps.
本發明人係經過無數次配方調整及無數次實作驗證，始獲得製作完成上述二氧化矽氣凝膠複合纖維毯的製造方法，其中，最關鍵的是該黏結劑配方的選擇，本發明針對該黏結劑選定由一有機黏結劑及一無機黏結劑混合組成，主要就是可以改善該改質濕矽氣凝膠與玻璃纖維毯間交互穿插的黏結性及物性；同時，本發明選定六甲基二矽氮烷為偶合劑及表面改質劑，可以增進該有機黏結劑與該無機黏結劑間的交聯反應及螯合作用，以及針對該玻璃纖維毯表面的疏水性改質，該六甲基二矽氮烷對於二氧化矽氣凝膠複合纖維毯(不論是二氧化矽氣凝膠玻璃纖維棉毯或二氧化矽氣凝膠玻璃纖維針軋毯)的密度、孔隙率、熱傳導係數及接觸角與掉粉量皆朝有利影響，最終可以製備出高強度(楊氏模數：0.09 ~ 0.58 MPa)、柔曲性佳(彎屈模數：0.04 ~ 0.05 MPa)、低熱傳導率(0.03 W/mK)、高疏水角(140o)，最重要是不掉粉的二氧化矽氣凝膠複合纖維毯。After countless formulation adjustments and countless actual verifications, the inventors have finally obtained the manufacturing method of the above-mentioned silica aerogel composite fiber blanket. Among them, the most important thing is the choice of the binder formula. The present invention is aimed at The bonding agent is selected to be composed of a mixture of an organic bonding agent and an inorganic bonding agent, mainly to improve the bonding and physical properties between the modified wet silica aerogel and the glass fiber blanket; at the same time, the present invention selects hexamethyl Disilazane is a coupling agent and a surface modifier, which can enhance the cross-linking reaction and chelating effect between the organic binder and the inorganic binder, as well as the hydrophobic modification of the surface of the glass fiber blanket. Based on the density, porosity, thermal conductivity and thermal conductivity of silica aerogel composite fiber blanket (whether it is silica aerogel glass fiber cotton blanket or silica aerogel glass fiber needle blanket) based on disilazane The contact angle and the amount of powder falling are both positively affected, and finally high strength (Young's modulus: 0.09 ~ 0.58 MPa), good flexibility (flexural modulus: 0.04 ~ 0.05 MPa), and low thermal conductivity (0.03 W/mK), high hydrophobic angle (140o), and the most important thing is the silica aerogel composite fiber blanket that does not drop powder.
由以上說明可知，本發明主要即先製備出一種性能優良的"改質濕矽氣凝膠"，再應用該"改質濕矽氣凝膠"進一步製造出一種耐高溫、絕熱性能佳，且不掉粉的"二氧化矽氣凝膠複合纖維毯"；本發明所製造出的"二氧化矽氣凝膠複合纖維毯"因為高強度，柔曲性佳、低熱傳導率，用來作為隔熱材料能獲致絕佳效果，尤其用來披覆於熱流體管路外壁上做為絕熱層時，可以隔絕流體管路的熱量散失，達致大幅節省能源之功效；同時可以阻絕所披覆管線壁面之腐蝕，達致節省檢視維修花費之功效。It can be seen from the above description that the present invention mainly firstly prepares a "modified wet silica aerogel" with excellent performance, and then uses the "modified wet silica aerogel" to further produce a high temperature resistance, thermal insulation performance, and The "silica aerogel composite fiber blanket" that does not drop powder; the "silica aerogel composite fiber blanket" manufactured by the present invention is used as a separator because of its high strength, good flexibility, and low thermal conductivity. Thermal materials can achieve excellent results, especially when used as a thermal insulation layer on the outer wall of the hot fluid pipeline, which can isolate the heat loss of the fluid pipeline and achieve a significant energy saving effect; at the same time, it can block the coated pipeline The corrosion of the wall can save the cost of inspection and maintenance.
於此必須加強說明的是，本發明係訴求先製備出一種性能優良的"改質濕矽氣凝膠"，再應用該"改質濕矽氣凝膠"進一步製造出一種耐高溫、絕熱性能佳，且不掉粉的"二氧化矽氣凝膠複合纖維毯"。這其中，該"改質濕矽氣凝膠"可以有二種來源：第一種即以上述步驟(6).所完成的"改質濕矽氣凝膠"(即不須經過常壓乾燥者)直接使用，以節省熱能成本；第二種則是在上述步驟(6).完成出"改質濕矽氣凝膠"後，有時為求大量儲存販賣或備用，製備上還會將該"改質濕矽氣凝膠"採行常壓乾燥法進行乾燥，例如：以60℃，150℃及230℃階梯式升溫方式各乾燥1小時，如此製備出"改質乾矽氣凝膠"。因此若取用該"改質乾矽氣凝膠"，然後加入於正已烷或相關醇類內浸置一段時間，例如：浸置於正已烷或甲醇、乙醇、異丙醇、丁醇或乙二醇---等，如此可令該"改質乾矽氣凝膠"回復成為"改質濕矽氣凝膠"。It must be emphasized here that the present invention seeks to first prepare a "modified wet silica aerogel" with excellent performance, and then use the "modified wet silica aerogel" to further produce a high temperature resistance and thermal insulation performance. Excellent, and no powder "silica aerogel composite fiber blanket". Among them, the "modified wet silica aerogel" can have two sources: the first is the "modified wet silica aerogel" completed in the above step (6) (that is, it does not need to be dried under normal pressure). (Or) to use directly to save thermal energy costs; the second is to complete the "modified wet silica aerogel" in the above step (6). Sometimes for mass storage and sale or backup, the preparation will also The "modified wet silica aerogel" is dried by the atmospheric drying method, for example: drying at 60°C, 150°C and 230°C for 1 hour each in a stepped heating manner, thus preparing the "modified dry silica aerogel" ". Therefore, if you take the "modified dry silica aerogel", then add it to n-hexane or related alcohols and soak for a period of time, for example: soak in n-hexane or methanol, ethanol, isopropanol, butanol Or ethylene glycol --- etc., so that the "modified dry silica aerogel" can be restored to a "modified wet silica aerogel".
因此不論是應用第一種來源的"改質濕矽氣凝膠"，或是應用第二種來源的"改質濕矽氣凝膠"，同樣可以進一步製造出耐高溫、絕熱性能佳，且不掉粉的"二氧化矽氣凝膠複合纖維毯"，達成本發明所預期之目的及功效。故縱係應用第二種來源的"改質濕矽氣凝膠"來製造出"二氧化矽氣凝膠複合纖維毯"，同樣會含括於本發明之專利權範圍內。Therefore, whether it is to use the "modified wet silica aerogel" from the first source or the "modified wet silica aerogel" from the second source, it can also be further manufactured with high temperature resistance and good thermal insulation performance. The powder-free "silica aerogel composite fiber blanket" achieves the intended purpose and effect of the invention. Therefore, the use of the second source of "modified wet silica aerogel" to produce a "silica aerogel composite fiber blanket" will also be included in the scope of the patent of the present invention.
綜上所述，本發明確可達到預期之功能及目的，並且詳細說明能使熟於此技藝者得據以實施，然以上所舉之實施例僅用以說明本發明，舉凡所有等效結構之改變仍不脫離本發明之專利範疇。In summary, the present invention clearly achieves the expected function and purpose, and the detailed description can enable those who are familiar with the art to implement it accordingly. However, the above-mentioned embodiments are only used to illustrate the present invention, and all equivalent structures are listed. The change still does not depart from the scope of the patent of the present invention.
(無)(without)
圖1所示係本發明之前端製備二氧化矽氣凝膠之步驟流程圖。 圖2所示係本發明之後端製造出二氧化矽氣凝膠複合纖維毯之步驟流程圖。Figure 1 shows a flow chart of the steps for preparing silica aerogel at the front end of the present invention. Fig. 2 shows a flow chart of the steps of manufacturing a silica aerogel composite fiber blanket at the back end of the present invention.
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