Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/65624
標題: 酚液化孟宗竹製備酚樹脂及其在成型材料製造之應用
Preparation of PF Resins from Phenol Liquefied Phyllostachys pubesens and Its Application in the Manufacturing of Moldings
作者: 陳奕君
Chen, Yi-Chun
關鍵字: liquefied moso bamboo
液化孟宗竹
PF resin
moldings
carbonized
酚樹脂
成型物
碳化
出版社: 森林學系
摘要: In this study, moso bamboo (Phyllostachys pubesens) was liquefied in phenol by using H2SO4 and HCl as catalyst, and the liquefied moso bamboos were used in the preparation of resol type water soluble PF resins, resol type alcohol soluble PF resin and novolak type PF resins. The synthesis condition of various PF resins and their manufacturing for moldings were investigated. These moldings were carbonized at 800℃ to prepare the carbon materials, and thermal property of these moldings were analyzed, too. Form the results, reaction temperature, kinds and concentration of catalyst and the ratio of phenol to bamboo (w/w) were all influence the liquefaction effect of moso bamboo. The best liquefaction condition was using the ratio of 3/1 of phenol to bamboo and 5 % of H2SO4(aq) and liquefied at 130 ℃ for 30 minutes, the residue of liquefied bamboo was only 1.3 %. FT-IR spectrum of liquefied bamboos showed that the chemical bonds had formed between phenol and components of bamboo. GPC analysis showed that liquefied bamboos had Mw between 1867~3550. When the liquefied bamboos was used in the preparation of resol type water soluble PF resins, bath the bind of liquefied bamboo and synthesis condition would influence the viscosity variation of resins at the stage of synthesis and gel time of prepared resins. When used in the manufacturing of plywood, C-1 that prepared from the liquefied with the ratio of 3/1 of phenol to bamboo (w/w) and using 10% of HCl as catalyst and liquefied at 120 ℃ for 60 minutes had the best bonding strength. The adequate synthesis conditions for resol type alcohol soluble PF resins made form liquefied bamboos were using the molar ratio of F/P 1.2/1 and ammonia solution of 10/1 (mL/mole). Before synthesis process, liquefied bamboo should mixed with formalin, 15g of 40 % NaOH(aq) and third ammonia solution, and then heating to 65 ℃ for 60 min, followed added the remain ammonia solution, and heating to 80 ℃ for 20~30 min. The molding of resol type alcohol soluble PF resins should be made by heating to 80 ℃ for 24 hr first, and then heating to 135 ℃ for 0.5 hr. The weight retention of these moldings after solvent resistance test was 92.5~99.7 %. Novolak type resin made form liquefied bamboos should be synthesized with the method used for RF resin. The weight retention of these moldings after solvent resistance test was 94.8~100.0 %. TGA analysis results showed that moldings made form resol type alcohol soluble PF resin had the highest char yield, and resol type water soluble was next, novolak resins is the lowest. Carbonization of various moldings with 800 ℃, the yield of moldings made form resol type alcohol soluble resins was highest, and the novolak type was next. The higher heating rate used the lower carbon yield would be.
本研究將孟宗竹材料在酚溶劑中以酸(硫酸、鹽酸)為催化劑進行液化處理,並將酚液化孟宗竹應用於Resol型水溶性、醇溶性及Novolak型酚樹脂之製備,探討各不同型態酚樹脂之合成條件及其成型物之製造條件,進一步將其成型物以800 ℃之高溫加熱製作碳材料,並分析其成型物之熱性質。由試驗結果得知,孟宗竹於酚溶液中進行液化處理時,反應溫度、酸催化劑種類與濃度及酚/竹材重量比均會影響其液化效果,其中以液比3/1,硫酸添加量5 %,並在130 ℃下反應60 min者具有最佳之液化效果,其殘渣率僅1.3 %。由FT-IR光譜分析圖顯示液化孟宗竹中酚與竹材組成分間產生鍵結。GPC分析顯示液化孟宗竹材之重量平均分子量介於1867~3550間。以液化孟宗竹製備Resol型水溶性酚樹脂時,試料種類及樹脂合成條件將影響其合成過程中樹脂液之經時黏度變化及合成樹脂之膠化時間,將其應用於合板膠合時,以酚/竹材重量比3/1,10 %HCl為液化催化劑,經120 ℃液化處理60 min之液化竹材所製備之C1-1有最佳的膠合強度。液化孟宗竹製備Resol型醇溶性酚樹脂之適用合成條件為F/P莫耳比1.2/1,氨水/P比例為10/1(ml/莫耳),合成時先將之酚液化竹材與福馬林混合,並添加40 % NaOH(aq)15 g及1/3量之氨水,隨後以60 min將反應液加熱至65 ℃,再加入剩餘之氨水,並在溫度80 ℃進行反應20~30 min,其合成樹脂之成型條件為80 ℃加熱24 hr,後以135 ℃加熱0.5 hr,成型物耐溶劑試驗之重量保留率介於92.5~99.7 %之間。液化孟宗竹製備Novolak型酚樹脂宜採用一般間苯二酚甲醛樹脂之合成法,其成型物耐溶劑性試驗之重量保留率介於94.8~100.0 %。各不同型態酚樹脂成型物之TGA熱分析結果顯示,Resol型醇溶性酚樹脂成型物之焦炭率最高,水溶性次之,Novolak型之最低。各成型物經800 ℃碳化處理後,以醇溶性酚樹脂之成型物有最高收率,其次為Novolak型酚樹脂,升溫速率較快,則碳化產物之收率較少。
URI: http://hdl.handle.net/11455/65624
Appears in Collections:森林學系

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